保留指数应用(8)----恒流和恒压模式下的保留指数对比
正构烷名称 | RI | RT(min) |
OCTANE | 800 | 4.126 |
PROPANONE | 810 | 4.078 |
NONANE | 900 | 4.756 |
DECANE | 1000 | 5.886 |
UNDECANE | 1100 | 7.742 |
DODECANE | 1200 | 10.410 |
TRIDECANE | 1300 | 13.765 |
TETRADECANE | 1400 | 17.533 |
PENTADECANE | 1500 | 21.449 |
HEXADECANE | 1600 | 25.353 |
HEPTADECANE | 1700 | 29.154 |
OCTADECANE | 1800 | 32.822 |
NONADECANE | 1900 | 36.343 |
EICOSANE | 2000 | 39.724 |
HENEICOSANE | 2100 | 42.966 |
DOCOSANE | 2200 | 46.069 |
TRICOSANE | 2300 | 49.059 |
TETRACOSANE | 2400 | 51.940 |
PENTACOSANE | 2500 | 54.713 |
HEXACOSANE | 2600 | 57.377 |
HEPTACOSANE | 2700 | 59.954 |
OCTACOSANE | 2800 | 62.449 |
NONACOSANE | 2900 | 64.948 |
TRIACONTANE | 3000 | 67.812 |
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正构烷名称 | RI | RT(min) |
OCTANE | 800 | 4.212 |
NONANE | 900 | 4.864 |
DECANE | 1000 | 6.041 |
UNDECANE | 1100 | 7.975 |
DODECANE | 1200 | 10.818 |
TRIDECANE | 1300 | 14.390 |
TETRADECANE | 1400 | 18.419 |
PENTADECANE | 1500 | 22.626 |
HEXADECANE | 1600 | 26.820 |
HEPTADECANE | 1700 | 30.905 |
OCTADECANE | 1800 | 34.803 |
NONADECANE | 1900 | 38.641 |
EICOSANE | 2000 | 42.278 |
HENEICOSANE | 2100 | 45.716 |
DOCOSANE | 2200 | 49.101 |
TRICOSANE | 2300 | 52.270 |
TETRACOSANE | 2400 | 55.403 |
PENTACOSANE | 2500 | 58.328 |
HEXACOSANE | 2600 | 61.196 |
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RT(min) | RI | RI | RT(min) | ||||
No | Compounds Name | 极性恒压 | 极性恒压 | 极性恒流 |
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1 | ETHYL ACETATE | 4.803 | 889 | 892 | 4.727 | ||
2 | ALCOHOL | 5.306 | 937 | 937 | 5.185 | ||
3 | ETHYL PROPIONATE | 5.576 | 959 | 961 | 5.484 | ||
4 | PINENE, ALPHA- | 6.598 | 1028 | 1028 | 6.415 | ||
5 | ETHYL BUTYRATE | 6.774 | 1037 | 1038 | 6.651 | ||
6 | CAMPHENE | 7.47 | 1073 | 1072 | 7.244 | ||
7 | PINENE, BETA- | 8.477 | 1117 | 1116 | 8.197 | ||
8 | MYRCENE | 9.82 | 1164 | 1164 | 9.471 | ||
9 | LIMONENE | 11.129 | 1208 | 1208 | 10.697 | ||
10 | ETHYL CAPRONATE | 12.099 | 1235 | 1236 | 11.744 | ||
11 | TERPINENE, GAMMA- | 12.63 | 1250 | 1250 | 12.105 | ||
12 | CYMENE, P- | 13.573 | 1276 | 1276 | 12.987 | ||
13 | HEXYL ACETATE | 13.5 | 1274 | 1276 | 13.07 | ||
14 | TERPINOLENE | 13.983 | 1288 | 1288 | 13.37 | ||
15 | ALDEHYDE C 8 | 14.224 | 1295 | 1294 | 13.601 | ||
16 | HEXENYL ACETATE, 3Z- | 15.223 | 1320 | 1322 | 14.7 | ||
17 | METHYL HEPTENONE, 6,5,2- | 16.093 | 1342 | 1343 | 15.507 | ||
18 | ALCOHOL C 6 | 16.463 | 1351 | 1352 | 15.849 | ||
19 | HEXENOL, 3E- | 16.936 | 1364 | 1364 | 16.304 | ||
20 | HEXENOL, 3Z- | 17.848 | 1385 | 1387 | 17.155 | ||
21 | ALDEHYDE C 9 | 18.381 | 1398 | 1398 | 17.478 | ||
22 | HEXENOL, 2E- | 18.688 | 1406 | 1408 | 17.944 | ||
23 | ACETIC ACID | 20.57 | 1450 | 1454 | 19.766 | ||
24 | LINALOOLOXIDE | 21.567 | 1475 | 1474 | 20.46 | ||
25 | CITRONELLAL | 21.972 | 1484 | 1483 | 20.82 | ||
26 | ALDEHYDE C10 | 22.72 | 1502 | 1502 | 21.563 | ||
27 | BENZALDEHYDE | 23.988 | 1532 | 1534 | 22.873 | ||
28 | PROPANOIC ACID | 24.299 | 1539 | 1543 | 23.238 | ||
29 | LINALOOL | 24.635 | 1547 | 1548 | 23.33 | ||
30 | DIETHYL MALONATE | 26.03 | 1580 | 1583 | 24.808 | ||
31 | PROPYLENE GLYCOL, 1,2- | 26.443 | 1590 | 1593 | 25.167 | ||
32 | CARYOPHYLLENE | 26.985 | 1603 | 1601 | 25.417 | ||
33 | ISOPHORONE | 26.943 | 1602 | 1602 | 25.539 | ||
34 | BUTYRIC ACID | 28.01 | 1628 | 1632 | 26.682 | ||
35 | CITRONELLYL ACETATE | 29.468 | 1664 | 1667 | 27.973 | ||
36 | NERAL | 30.464 | 1688 | 1687 | 28.678 | ||
37 | TERPINEOL, ALPHA- | 30.717 | 1700 | 1698 | 29.117 | ||
38 | STYROLYL ACETATE | 31.38 | 1706 | 1709 | 29.566 | ||
39 | NERYL ACETATE | 32.096 | 1730 | 1729 | 30.23 | ||
40 | GERANIAL | 32.485 | 1740 | 1738 | 30.56 | ||
41 | BENZYL ACETATE | 32.291 | 1735 | 1737 | 30.592 | ||
42 | GERANYL ACETATE | 33.254 | 1759 | 1758 | 31.31 | ||
43 | CITRONELLOL | 33.497 | 1766 | 1768 | 31.733 | ||
44 | NEROL | 34.886 | 1801 | 1799 | 32.829 | ||
45 | PHENYLETHYL ACETATE, 2- | 35.688 | 1822 | 1824 | 33.725 | ||
46 | GERANIOL | 36.626 | 1847 | 1846 | 34.46 | ||
47 | CAPRONIC ACID | 36.574 | 1845 | 1850 | 34.634 | ||
48 | PHENYLETHYL ALCOHOL, 2- | 39.201 | 1914 | 1918 | 36.99 | ||
49 | MALTOL | 41.189 | 1969 | 1971 | 38.79 | ||
50 | FURANEOL | 43.491 | 2035 | 2039 | 41.001 | ||
51 | TRIACETIN | 44.942 | 2077 | 2076 | 42.199 | ||
52 | THYMOL | 48.577 | 2183 | 2183 | 45.552 | ||
53 | METHYL ANTHRANILATE | 50.677 | 2249 | 2251 | 47.581 | ||
54 | GERANIC ACID | 53.446 | 2337 | 2335 | 50.074 |
恒流 | 恒流 | 恒压 |
| 差值 | ||||
No | Compounds Name | Time | RI | RI | Time | 恒压-恒流 | ||
1 | ETHYL PROPIONATE | 2.325 | 710 | 709 | 2.364 | -1 | ||
2 | PROPYLENE GLYCOL, 1,2- | 2.53 | 732 | 728 | 2.526 | -4 | ||
3 | ETHYL ISOBUTYRATE | 2.671 | 752 | 751 | 2.721 | -1 | ||
4 | BUTYRIC ACID | 3.207 | 810 | 787 | 3.019 | -23 | ||
5 | ETHYL BUTYRATE | 3.138 | 801 | 799 | 3.138 | -2 | ||
6 | HEXENOL, 3Z- | 3.819 | 854 | 850 | 3.873 | -4 | ||
7 | HEXENOL, 2E- | 3.919 | 861 | 859 | 4.003 | -2 | ||
8 | ALCOHOL C 6 | 3.948 | 863 | 861 | 4.03 | -2 | ||
9 | BENZALDEHYDE | 5.626 | 958 | 958 | 5.807 | 0 | ||
10 | CAPRONIC ACID | 6.131 | 983 | 973 | 6.136 | -10 | ||
11 | METHYL HEPTENONE, 6,5,2- | 6.131 | 983 | 983 | 6.339 | 0 | ||
12 | ETHYL CAPRONATE | 6.41 | 997 | 996 | 6.625 | -1 | ||
13 | HEXENYL ACETATE, 3Z- | 6.582 | 1004 | 1004 | 6.805 | 0 | ||
14 | HEXYL ACETATE | 6.723 | 1010 | 1010 | 6.955 | 0 | ||
15 | FURANEOL | 7.698 | 1050 | 1048 | 7.934 | -2 | ||
16 | DIETHYL MALONATE | 8.07 | 1066 | 1065 | 8.365 | -1 | ||
17 | LINALOOL | 8.894 | 1099 | 1099 | 9.24 | 0 | ||
18 | MALTOL | 9.139 | 1109 | 1108 | 9.514 | -1 | ||
19 | PHENYLETHYL ALCOHOL, 2- | 9.214 | 1112 | 1112 | 9.582 | 0 | ||
20 | ISOPHORONE | 9.43 | 1120 | 1120 | 9.822 | 0 | ||
21 | BENZYL ACETATE | 10.535 | 1162 | 1161 | 10.992 | -1 | ||
22 | STYROLYL ACETATE | 11.368 | 1194 | 1192 | 11.851 | -2 | ||
23 | PHENYLETHYL ACETATE, 2- | 12.997 | 1255 | 1255 | 13.601 | 0 | ||
24 | METHYL ANTHRANILATE | 15.39 | 1348 | 1344 | 16.055 | -4 | ||
25 | CITRONELLYL ACETATE | 15.522 | 1353 | 1351 | 16.26 | -2 |
原文由 symmacros(jimzhu) 发表:2.3 非极性柱子恒流恒压模式正构烷标样结果在上述1.3的相同条件下,进C7-C30或C6-C26正构烷烃标样,得到其保留时间,用于计算其它化合物的保留指数。图3 非极性柱子,恒流模式,60℃,以3 ℃/min升至250℃的正构烷(C8-C30)总离子色谱图TIC图4 非极性柱子,恒压模式,60℃,以3 ℃/min升至250℃的正构烷(C7-C26)总离子色谱图TIC**************************************************************************************************和极性柱子情况一样,由于恒压模式下流量随着柱温升高而下降,从柱温60度到250度流量从1.9ml/min下降到约0.6ml/min,从而分离时间加长不少,出峰慢一些。例如C26在恒流模式下在39.952min出峰,而在恒压模式下在42.927min出峰。2.4. 非极性柱子恒流恒压模式保留指数的对比部分香气化合物的保留指数(非极性柱子)结果用和极性柱子同样的计算方法来计算化合物的保留指数如下: 恒流恒流恒压 恒压差值NoCompounds NameTimeRIRITime恒压-恒流1ETHYL PROPIONATE2.3257107092.364-12PROPYLENE GLYCOL, 1,2-2.537327282.526-43ETHYL ISOBUTYRATE2.6717527512.721-14BUTYRIC ACID3.2078107873.019-235ETHYL BUTYRATE3.1388017993.138-26HEXENOL, 3Z-3.8198548503.873-47HEXENOL, 2E-3.9198618594.003-28ALCOHOL C 63.9488638614.03-29BENZALDEHYDE5.6269589585.807010CAPRONIC ACID6.1319839736.136-1011METHYL HEPTENONE, 6,5,2-6.1319839836.339012ETHYL CAPRONATE6.419979966.625-113HEXENYL ACETATE, 3Z-6.582100410046.805014HEXYL ACETATE6.723101010106.955015FURANEOL7.698105010487.934-216DIETHYL MALONATE8.07106610658.365-117LINALOOL8.894109910999.24018MALTOL9.139110911089.514-119PHENYLETHYL ALCOHOL, 2-9.214111211129.582020ISOPHORONE9.43112011209.822021BENZYL ACETATE10.5351162116110.992-122STYROLYL ACETATE11.3681194119211.851-223PHENYLETHYL ACETATE, 2-12.9971255125513.601024METHYL ANTHRANILATE15.391348134416.055-425CITRONELLYL ACETATE15.5221353135116.26-2从上面看非极性柱子在恒流和恒压两种模式的保留指数有一定的变化,但一般变化非常小。酸类化合物变化比较大一些,差异较大。特别是丁酸差值为23。观察色谱图的分离情况,恰好在这个位置丁酸的另外的化合物分离变化较大,和丁酸乙酯的位置对调,前后发生变化在恒压时候分离更好。其它化合物这种小的差异不影响两种模式的保留指数的转换和定性。和极性柱子的结果一样,恒流和恒压的保留指数差别更小(酸类化合物除外)。本次实验(非极性柱子)共测定了约400多种化合物的保留指数,结果基本和上面一致,差别很小。另外恒压的分离效果似乎比恒流效果要好一些,这是可能因为恒压的流速相对低一些。不同结构、不同性质、不同极性、不同沸点的化合物的定向力、诱导力、色散力、氢键作用力都不同。在色谱柱的温度变化(升温速率不同)时候,这些力中有些占主导作用并随条件改变而改变,可以会产生不同影响。正构烷是非极性化合物,与有些其它化合物的极性可能不同,在色谱柱中迁移快慢有所不同。条件改变时候可能会有一定的影响。会造成极性强的酸类化合物在非极性柱子的恒流和恒压模式的保留指数变化更大。有空好好读一下 ,横压法现在还没有搞定 暂时用ri