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【求助】色谱柱和柱温的关系?

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  • 液相用色谱柱的柱温升高,对保留时间的影响是怎么样的呢?
    先听听大家的说法,再和大家说说我的实际情况,最近的实验很反常!
  • 该帖子已被版主-月旭科技--小S加10积分,加2经验;加分理由:鼓励来本版发求助帖!
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  • 1234chen

    第1楼2009/12/10

    在我的一些实验中,是柱温高了,时间提前。不知你的实验是怎么反常?

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  • freewsb2003

    第2楼2009/12/10

    我们做样品时升高柱温,保留时间一般情况下是缩短,还没见过延长的情况

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  • jcj9803

    第5楼2009/12/10

    最好是能用上柱温箱

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  • pheui

    第6楼2009/12/10

    一般情况下,柱温升高,保留时间变短。但是我在论坛上见过有人说,温度升高,保留时间变长:是用四元泵需要二(三)相溶剂混合的时候,发现当室温突然变化,由于四元泵的溶剂部分都没有保温,引起溶剂密度的变化,进而引起实际的溶剂配比发生变化。不过这个没有亲自验证过……还请达人指教!!

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  • plexu

    第7楼2009/12/10

    Myth 4: High Temperature Always Leads to Better Separations

    False. As the temperature increases, the viscosity of the mobile phase decreases and therefore the rate of solute mass transfer should increase thereby offering better chromatographic efficiency. True, but besides the column efficiency term (H), temperature also can affect the retention factor (k) and selectivity (α). The impact on these terms can result in improved resolution (which is really what we are concerned about in chromatography) or detract from it. Retention usually decreases as the temperature increases because, being a thermodynamic parameter, the analyte prefers to remain in the mobile phase and are eluted sooner from the column. However, different chemical species might have different degrees of change in their retention versus temperature. Stated more correctly, their van''t Hoff plots (ln k vs. 1/T where the temperature T is measured in kelvins) might display different slopes; in other words, their α values can change. In addition, high temperature can cause a low k peak to be eluted so quickly that it can be eluted at or near t , the unretained peak retention time, and therefore be difficult to quantitate. .
    Take the example of analgesics shown in Figure 2. This series of chromatograms shows the separation of seven analgesics at column temperatures of 20–90 °C. One can note several features of the chromatograms. First, the retention of all peaks is decreased with higher temperatures and the peaks do become narrower indicating improved efficiency. Second, one of the analgesic compounds, salicylic acid, has a much greater retention change with temperature relative to peaks 5 and 6, the closest eluted compounds. In fact, the elution order is reversed after increasing the temperature from 20 to 40 °C. At the intermediate 30 °C temperature, the salicylic acid and peak number 6, phenacetin, are coeluted. So in this case, temperatures greater than 40 °C resulted in a shorter separation time for the entire separation yet the elution order was changed from the lower temperatures.
    Of course, a side benefit of operating at higher temperature is the decrease in column operating pressure that allows one to use higher flow rates or smaller particles.
    Another experimental parameter that can cause column performance problems at higher temperature is the possible thermal mismatch of the incoming mobile phase. For example, if the column is heated to 60 °C and the incoming solvent is at room temperature, the incoming cooler solvent can cause peaks to be distorted because of the differences in the temperature that the solutes can experience in the initial part of the column. It is recommended that one preheats the mobile phase when using higher column temperatures

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  • plexu

    第8楼2009/12/10

    关于柱温和色谱分离的关系,十大神话里的上面这部分有很好的解释.

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  • 楚无伤

    第9楼2009/12/10

    保留时间会提前的说
    前提是你整个温度系统是稳定的

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  • 1234chen

    第10楼2009/12/10

    PLEXU 的图很形象、直观。

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