- 注册时间
- 2012-10-15
- 最后登录
- 2020-6-22
- 阅读权限
- 200
- 积分
- 242
- 精华
- 0
- 帖子
- 57
|
一.载气流量的测定
色谱载气流量多用体积流量表示,可用皂膜流量计测定.
皂膜流量计是一个内径均匀,下端为三通管的玻璃叉管,三通叉管底部连接盛有十二烷基磺酸钠水溶液的橡皮滴头,三通叉管的侧管在接色谱柱出口,测量时将载气连续地从侧管通入,然后手捏底部橡皮滴头,使气流顶着皂膜通过刻度管所需时间,经过计算,就可得出柱出口温度和压力(含饱和水蒸气压),皂膜流量计刻度管的校正方法与校正滴定管的方法相同,皂膜流量计能够很精确的测定(1-50)ml?min-1的气体流量,使用时能将内壁洗净、湿润、检查管路有无漏气,以免产生误差。
二.载气流量的校正
欲将在色谱柱(或检测器)后用连接皂膜流量计测量所得的视体和流量Fo,换算成色谱柱操作条件下的流量F,则需要作如下三种校正,
1.水蒸气校正
由于载气通过皂膜流量计时,被室温的水蒸气饱和,测定的流量Fo是被水蒸气饱和的载气的流量,故在柱出口的温度(K)和压力(不含饱和水蒸气压)的实际体积流量Fa的值为:
Po-Pn
Fa=Fo? ------------??
Po
式中,Po是大气压力,Pa:Pn是测量时定温下水的饱和蒸气压,Pa,水蒸气饱和蒸气压见表。
水 蒸 气 饱 和 蒸 汽 压
| (单位mmHg)① | 温度/℃ | 0.0 | 0.2 | 0.4 | 0.6 | 0.8 | 温度/℃ | 0.0 | 0.2 | 0.4 | 0.6 | 0.8 | 0 | 4.579 | 4.647 | 4.715 | 4.785 | 4.855 | 21 | 18.650 | 18.880 | 19.113 | 19.349 | 19.587 | 1 | 4.926 | 4.998 | 5.070 | 5.144 | 5.219 | 22 | 19.827 | 20.070 | 20.316 | 20.565 | 20.815 | 2 | 5.294 | 5.370 | 5.447 | 5.525 | 5.605 | 23 | 21.068 | 21.324 | 21.583 | 21.845 | 22.110 | 3 | 5.685 | 5.766 | 5.848 | 5.931 | 6.015 | 24 | 22.377 | 22.648 | 22.922 | 23.198 | 23.476 | 4 | 6.101 | 6.187 | 6.274 | 6.363 | 6.453 | 25 | 23.756 | 24.039 | 24.326 | 24.617 | 24.912 | 5 | 6.543 | 6.635 | 6.728 | 6.822 | 6.917 | 26 | 25.209 | 25.509 | 25.812 | 26.117 | 26.426 | 6 | 7.013 | 7.111 | 7.209 | 7.309 | 7.411 | 27 | 26.739 | 27.055 | 27.374 | 27.696 | 28.021 | 7 | 7.513 | 7.617 | 7.722 | 7.828 | 7.936 | 28 | 28.349 | 28.680 | 29.015 | 29.354 | 29.617 | 8 | 8.045 | 8.155 | 8.267 | 8.380 | 8.494 | 29 | 30.043 | 30.392 | 30.745 | 31.102 | 31.461 | 9 | 8.609 | 8.727 | 8.845 | 8.965 | 9.086 | 30 | 31.824 | 32.191 | 32.561 | 32.934 | 33.312 | 10 | 9.209 | 9.333 | 9.458 | 9.585 | 9.714 | 31 | 33.695 | 34.082 | 34.471 | 34.864 | 35.261 | 11 | 9.844 | 9.976 | 10.109 | 10.244 | 10.380 | 32 | 35.663 | 36.068 | 36.477 | 36.891 | 37.308 | 12 | 10.518 | 10.658 | 10.799 | 10.941 | 11.085 | 33 | 37.729 | 38.155 | 38.584 | 39.018 | 39.457 | 13 | 11.231 | 11.379 | 11.528 | 11.680 | 11.833 | 34 | 39.898 | 40.344 | 40.796 | 41.251 | 41.710 | 14 | 11.987 | 12.144 | 12.302 | 12.462 | 12.624 | 35 | 42.175 | 42.644 | 43.117 | 43.595 | 44.078 | 15 | 12.788 | 12.953 | 13.121 | 13.290 | 13.461 | 36 | 44.563 | 45.054 | 45.549 | 46.050 | 46.556 | 16 | 13.634 | 13.809 | 13.987 | 14.166 | 14.347 | 37 | 47.067 | 47.582 | 48.102 | 48.627 | 49.157 | 17 | 14.530 | 14.715 | 14.903 | 15.092 | 15.284 | 38 | 49.692 | 50.231 | 50.774 | 51.323 | 51.879 | 18 | 15.477 | 15.673 | 15.871 | 16.071 | 16.272 | 39 | 52.442 | 53.009 | 53.580 | 54.156 | 54.737 | 19 | 16.477 | 16.685 | 16.894 | 17.105 | 17.319 | 40 | 55.324 | 55.91 | 56.51 | 57.11 | 57.72 | 20 | 17.535 | 17.753 | 17.974 | 18.197 | 18.422 | | | | | | | ①1mmHg = 133.3Pa | | | | | | | | | |
2.温度的校正
经过水蒸气分压校正的载气流量Fa是柱出口温度(定温)和压力下的载气流量,需要校正的柱温(炉温)的载气校正体积流量:
Tc
Fc=Fa? ------------??
Ta
式中,Ta是柱出口温度,单位为K,Tc是柱温,单位为K。
3.压力校正
经过水蒸气分压和温度校正后的流量Fc成为载气在柱出口的压力(大气压力)测定的流量,还需要校正到柱的平均压力下的载气平均体积流量。
F=Fc?J
式中,J是色谱柱压力梯度校正因子,可由下式求出:
2007-9-23 15:29:12 上传
下载附件 (6.79 KB)
jpg
式中,Pi与Po分别式载气在色谱柱出口与柱出的绝对压力,J值也可以由压力梯度校正因子表查得。
压力梯度校正因子(j)
| pi
po
| 0.00 | 0.01 | 0.02 | 0.03 | 0.04 | 0.05 | 0.06 | 0.07 | 0.08 | 0.09 | 6.00 | 0.2442 | — | — | — | — | — | — | — | — | — | 1.00 | 1.000 | 0.9950 | 0.9900 | 0.9851 | 0.9803 | 0.9754 | 0.9706 | 0.9658 | 0.9611 | 0.9563 | 1.10 | 0.9517 | 0.9470 | 0.9424 | 0.9378 | 0.9333 | 0.9287 | 0.9242 | 0.9198 | 0.9154 | 0.9110 | 1.20 | 0.9066 | 0.9023 | 0.8980 | 0.8937 | 0.8895 | 0.8853 | 0.8811 | 0.8769 | 0.8728 | 0.8687 | 1.30 | 0.8646 | 0.8606 | 0.8566 | 0.8527 | 0.8487 | 0.8447 | 0.8408 | 0.8371 | 0.8333 | 0.8295 | 1.40 | 0.8257 | 0.8219 | 0.8182 | 0.8145 | 0.8109 | 0.8073 | 0.8037 | 0.8001 | 0.7965 | 0.7930 | 1.50 | 0.7895 | 0.7860 | 0.7825 | 0.7791 | 0.7757 | 0.7727 | 0.7690 | 0.7657 | 0.7624 | 0.7591 | 1.60 | 0.7558 | 0.7526 | 0.7494 | 0.7462 | 0.7430 | 0.7399 | 0.7368 | 0.7337 | 0.7306 | 0.7275 | 1.70 | 0.7245 | 0.7215 | 0.7185 | 0.7155 | 0.7126 | 0.7097 | 0.7068 | 0.7039 | 0.7010 | 0.6982 | 1.80 | 0.6954 | 0.6926 | 0.6898 | 0.6870 | 0.6843 | 0.6815 | 0.6788 | 0.6762 | 0.6735 | 0.6708 | 1.90 | 0.6682 | 0.6656 | 0.6630 | 0.6604 | 0.6579 | 0.6553 | 0.6528 | 0.6503 | 0.6478 | 0.6453 | 2.00 | 0.6429 | 0.6404 | 0.6380 | 0.6356 | 0.6332 | 0.6308 | 0.6285 | 0.6261 | 0.6238 | 0.6215 | 2.10 | 0.6192 | 0.6169 | 0.6146 | 0.6124 | 0.6101 | 0.6079 | 0.6057 | 0.6035 | 0.6013 | 0.5992 | 2.20 | 0.5970 | 0.5949 | 0.5928 | 0.5906 | 0.5885 | 0.5865 | 0.5844 | 0.5823 | 0.5803 | 0.5783 | 2.30 | 0.5763 | 0.5742 | 0.5723 | 0.5703 | 0.5683 | 0.5664 | 0.5644 | 0.5625 | 0.5606 | 0.5587 | 2.40 | 0.5568 | 0.5549 | 0.5530 | 0.5512 | 0.5493 | 0.5475 | 0.5465 | 0.5438 | 0.5420 | 0.5402 | 2.50 | 0.5385 | 0.5367 | 0.5349 | 0.5332 | 0.5314 | 0.5297 | 0.5280 | 0.5263 | 0.5246 | 0.5229 | 2.60 | 0.5212 | 0.5196 | 0.5179 | 0.5163 | 0.5146 | 0.5130 | 0.5114 | 0.5098 | 0.5082 | 0.5065 | 2.70 | 0.5050 | 0.5034 | 0.5019 | 0.5003 | 0.4988 | 0.4972 | 0.4957 | 0.4942 | 0.4927 | 0.4912 | 2.80 | 0.4897 | 0.4882 | 0.4867 | 0.4852 | 0.4838 | 0.4824 | 0.4809 | 0.4795 | 0.4781 | 0.4766 | 2.90 | 0.4752 | 0.4738 | 0.4724 | 0.4710 | 0.4697 | 0.4683 | 0.4669 | 0.4656 | 0.4643 | 0.4629 | 3.00 | 0.4615 | 0.4602 | 0.4589 | 0.4576 | 0.4563 | 0.4550 | 0.4537 | 0.4523 | 0.4511 | 0.4499 | 3.10 | 0.4486 | 0.4473 | 0.4461 | 0.4448 | 0.4436 | 0.4424 | 0.4411 | 0.4399 | 0.4387 | 0.4375 | 3.20 | 0.4363 | 0.4351 | 0.4340 | 0.4328 | 0.4316 | 0.4304 | 0.4293 | 0.4281 | 0.4269 | 0.4258 | 3.30 | 0.4247 | 0.4235 | 0.4223 | 0.4212 | 0.4202 | 0.4190 | 0.4179 | 0.4169 | 0.4157 | 0.4146 | 3.40 | 0.4136 | 0.4122 | 0.4115 | 0.4101 | 0.4092 | 0.4082 | 0.4071 | 0.4061 | 0.4050 | 0.4040 | 3.50 | 0.4031 | 0.4020 | 0.4010 | 0.3999 | 0.3989 | 0.3980 | 0.3969 | 0.3959 | 0.3950 | 0.3939 | 3.60 | 0.3930 | 0.3920 | 0.3910 | 0.3900 | 0.3891 | 0.3881 | 0.3872 | 0.3863 | 0.3852 | 0.3843 | 3.70 | 0.3834 | 0.3824 | 0.3815 | 0.3806 | 0.3797 | 0.3787 | 0.3778 | 0.3769 | 0.3760 | 0.3751 | 3.80 | 0.3743 | 0.3734 | 0.3724 | 0.3716 | 0.3707 | 0.3698 | 0.3689 | 0.3681 | 0.3672 | 0.3664 | 3.90 | 0.3656 | 0.3647 | 0.3638 | 0.3629 | 0.3621 | 0.3612 | 0.3605 | 0.3596 | 0.3588 | 0.3580 | 4.00 | 0.3572 | 0.3564 | 0.3555 | 0.3548 | 0.3539 | 0.3531 | 0.3523 | 0.3515 | 0.3507 | 0.3500 | 4.10 | 0.3492 | 0.3481 | 0.3476 | 0.3468 | 0.3461 | 0.3453 | 0.3445 | 0.3438 | 0.3431 | 0.3423 | 4.20 | 0.3416 | 0.3408 | 0.3401 | 0.3393 | 0.3385 | 0.3378 | 0.3371 | 0.3363 | 0.3356 | 0.3350 | 4.30 | 0.3342 | 0.3335 | 0.3328 | 0.3321 | 0.3314 | 0.3306 | 0.3300 | 0.3295 | 0.3285 | 0.3278 | 4.40 | 0.3271 | 0.3265 | 0.3258 | 0.3251 | 0.3245 | 0.3237 | 0.3231 | 0.3224 | 0.3217 | 0.3211 | 4.50 | 0.3204 | 0.3198 | 0.3191 | 0.3185 | 0.3178 | 0.3171 | 0.3165 | 0.3158 | 0.3152 | 0.3146 | 4.60 | 0.3140 | 0.3132 | 0.3126 | 0.3120 | 0.3114 | 0.3108 | 0.3101 | 0.3095 | 0.3089 | 0.3083 | 4.70 | 0.3077 | 0.3071 | 0.3065 | 0.3059 | 0.3052 | 0.3046 | 0.3040 | 0.3034 | 0.3029 | 0.3025 | 4.80 | 0.3017 | 0.3011 | 0.3005 | 0.2999 | 0.2994 | 0.2987 | 0.2982 | 0.2976 | 0.2970 | 0.2964 | 4.90 | 0.2960 | 0.2954 | 0.2948 | 0.2942 | 0.2937 | 0.2931 | 0.2925 | 0.2919 | 0.2915 | 0.2909 | 5.00 | 0.2903 | 0.2898 | 0.2892 | 0.2888 | 0.2882 | 0.2876 | 0.2871 | 0.2866 | 0.2860 | 0.2855 | 5.10 | 0.2850 | 0.2844 | 0.2840 | 0.2834 | 0.2829 | 0.2823 | 0.2819 | 0.2813 | 0.2808 | 0.2803 | 5.20 | 0.2798 | 0.2793 | 0.2787 | 0.2783 | 0.2778 | 0.2772 | 0.2768 | 0.2762 | 0.2757 | 0.2753 | 5.30 | 0.2748 | 0.2743 | 0.2738 | 0.2733 | 0.2729 | 0.2724 | 0.2719 | 0.2714 | 0.2709 | 0.2704 | 5.40 | 0.2700 | 0.2695 | 0.2690 | 0.2685 | 0.2681 | 0.2676 | 0.2672 | 0.2667 | 0.2663 | 0.2658 | 5.50 | 0.2654 | 0.2649 | 0.2645 | 0.2640 | 0.2636 | 0.2631 | 0.2627 | 0.2621 | 0.2618 | 0.2612 | 5.60 | 0.2608 | 0.2604 | 0.2600 | 0.2595 | 0.2591 | 0.2586 | 0.2582 | 0.2577 | 0.2573 | 0.2568 | 5.70 | 0.2564 | 0.2561 | 0.2556 | 0.2552 | 0.2548 | 0.2543 | 0.2540 | 0.2535 | 0.2531 | 0.2526 | 5.80 | 0.2523 | 0.2519 | 0.2514 | 0.2510 | 0.2507 | 0.2502 | 0.2498 | 0.2494 | 0.2490 | 0.2486 | 5.90 | 0.2482 | 0.2478 | 0.2474 | 0.2469 | 0.2466 | 0.2452 | 0.2457 | 0.2454 | 0.2450 | 0.2446 |
顺便指出,若用Uo表示柱出口处载气线速,则有
Fa
Uo=-----??
? eq
式中e为柱内颗粒得孔隙率,q式柱的横截面积,当色谱柱是涂壁空心柱时,固?=1,则有
Fa
Uo=-----??
q
用色谱柱压力梯度校正因子校正的压缩性,柱内载气的平均速度为
?u'=JUo |
|