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关于皂膜流量计

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发表于 2012-10-15 11:35:55 |只看该作者 |倒序浏览
最近从贵公司购买了皂膜流量计,但不知道如何使用,请告之。
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发表于 2012-10-15 11:37:06 |只看该作者

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)
温度/0.00.20.40.60.8温度/0.00.20.40.60.8
04.5794.6474.7154.7854.8552118.65018.88019.11319.34919.587
14.9264.9985.0705.1445.2192219.82720.07020.31620.56520.815
25.2945.3705.4475.5255.6052321.06821.32421.58321.84522.110
35.6855.7665.8485.9316.0152422.37722.64822.92223.19823.476
46.1016.1876.2746.3636.4532523.75624.03924.32624.61724.912
56.5436.6356.7286.8226.9172625.20925.50925.81226.11726.426
67.0137.1117.2097.3097.4112726.73927.05527.37427.69628.021
77.5137.6177.7227.8287.9362828.34928.68029.01529.35429.617
88.0458.1558.2678.3808.4942930.04330.39230.74531.10231.461
98.6098.7278.8458.9659.0863031.82432.19132.56132.93433.312
109.2099.3339.4589.5859.7143133.69534.08234.47134.86435.261
119.8449.97610.10910.24410.3803235.66336.06836.47736.89137.308
1210.51810.65810.79910.94111.0853337.72938.15538.58439.01839.457
1311.23111.37911.52811.68011.8333439.89840.34440.79641.25141.710
1411.98712.14412.30212.46212.6243542.17542.64443.11743.59544.078
1512.78812.95313.12113.29013.4613644.56345.05445.54946.05046.556
1613.63413.80913.98714.16614.3473747.06747.58248.10248.62749.157
1714.53014.71514.90315.09215.2843849.69250.23150.77451.32351.879
1815.47715.67315.87116.07116.2723952.44253.00953.58054.15654.737
1916.47716.68516.89417.10517.3194055.32455.9156.5157.1157.72
2017.53517.75317.97418.19718.422      
      1mmHg = 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
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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

 
0.000.010.020.030.040.050.060.070.080.09
6.000.2442
1.001.0000.99500.99000.98510.98030.97540.97060.96580.96110.9563
1.100.95170.94700.94240.93780.93330.92870.92420.91980.91540.9110
1.200.90660.90230.89800.89370.88950.88530.88110.87690.87280.8687
1.300.86460.86060.85660.85270.84870.84470.84080.83710.83330.8295
1.400.82570.82190.81820.81450.81090.80730.80370.80010.79650.7930
1.500.78950.78600.78250.77910.77570.77270.76900.76570.76240.7591
1.600.75580.75260.74940.74620.74300.73990.73680.73370.73060.7275
1.700.72450.72150.71850.71550.71260.70970.70680.70390.70100.6982
1.800.69540.69260.68980.68700.68430.68150.67880.67620.67350.6708
1.900.66820.66560.66300.66040.65790.65530.65280.65030.64780.6453
2.000.64290.64040.63800.63560.63320.63080.62850.62610.62380.6215
2.100.61920.61690.61460.61240.61010.60790.60570.60350.60130.5992
2.200.59700.59490.59280.59060.58850.58650.58440.58230.58030.5783
2.300.57630.57420.57230.57030.56830.56640.56440.56250.56060.5587
2.400.55680.55490.55300.55120.54930.54750.54650.54380.54200.5402
2.500.53850.53670.53490.53320.53140.52970.52800.52630.52460.5229
2.600.52120.51960.51790.51630.51460.51300.51140.50980.50820.5065
2.700.50500.50340.50190.50030.49880.49720.49570.49420.49270.4912
2.800.48970.48820.48670.48520.48380.48240.48090.47950.47810.4766
2.900.47520.47380.47240.47100.46970.46830.46690.46560.46430.4629
3.000.46150.46020.45890.45760.45630.45500.45370.45230.45110.4499
3.100.44860.44730.44610.44480.44360.44240.44110.43990.43870.4375
3.200.43630.43510.43400.43280.43160.43040.42930.42810.42690.4258
3.300.42470.42350.42230.42120.42020.41900.41790.41690.41570.4146
3.400.41360.41220.41150.41010.40920.40820.40710.40610.40500.4040
3.500.40310.40200.40100.39990.39890.39800.39690.39590.39500.3939
3.600.39300.39200.39100.39000.38910.38810.38720.38630.38520.3843
3.700.38340.38240.38150.38060.37970.37870.37780.37690.37600.3751
3.800.37430.37340.37240.37160.37070.36980.36890.36810.36720.3664
3.900.36560.36470.36380.36290.36210.36120.36050.35960.35880.3580
4.000.35720.35640.35550.35480.35390.35310.35230.35150.35070.3500
4.100.34920.34810.34760.34680.34610.34530.34450.34380.34310.3423
4.200.34160.34080.34010.33930.33850.33780.33710.33630.33560.3350
4.300.33420.33350.33280.33210.33140.33060.33000.32950.32850.3278
4.400.32710.32650.32580.32510.32450.32370.32310.32240.32170.3211
4.500.32040.31980.31910.31850.31780.31710.31650.31580.31520.3146
4.600.31400.31320.31260.31200.31140.31080.31010.30950.30890.3083
4.700.30770.30710.30650.30590.30520.30460.30400.30340.30290.3025
4.800.30170.30110.30050.29990.29940.29870.29820.29760.29700.2964
4.900.29600.29540.29480.29420.29370.29310.29250.29190.29150.2909
5.000.29030.28980.28920.28880.28820.28760.28710.28660.28600.2855
5.100.28500.28440.28400.28340.28290.28230.28190.28130.28080.2803
5.200.27980.27930.27870.27830.27780.27720.27680.27620.27570.2753
5.300.27480.27430.27380.27330.27290.27240.27190.27140.27090.2704
5.400.27000.26950.26900.26850.26810.26760.26720.26670.26630.2658
5.500.26540.26490.26450.26400.26360.26310.26270.26210.26180.2612
5.600.26080.26040.26000.25950.25910.25860.25820.25770.25730.2568
5.700.25640.25610.25560.25520.25480.25430.25400.25350.25310.2526
5.800.25230.25190.25140.25100.25070.25020.24980.24940.24900.2486
5.900.24820.24780.24740.24690.24660.24520.24570.24540.24500.2446


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
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