怎么调整活动相完成提高别离度与改进峰形

版块：机械制造类型：普通作者：化工产业技术分享查看：77 回复：0 获赞：0 时间：2022-05-18 17:56:35

昨日的别离度不太行呀，活动相要再调调！”这话是不是很熟悉？调调？！咋调？假如你还不知道怎么制造适宜的活动相瞅这儿！

诀窍1：由强到弱

一般先用90%的乙腈(或甲醇)/水(或缓冲溶液)进行实验，这样能够很快地得到别离成果，然后依据出峰状况调整有机溶剂(乙腈或甲醇)的份额。

诀窍2：三倍规矩

每削减10%的有机溶剂(甲醇或乙腈)的量，保存因子约添加3倍，此为三倍规矩。这是一个聪明而又省力的方法。调整的过程中，留意调查各个峰的别离状况。

诀窍3：粗调转微调

当别离到达必定程度，应将有机溶剂10%的改动量调整为5%，并据此规矩逐步下降调整率，直至各组分的别离状况不再改动。

1．活动相的性质要求一个抱负的液相色谱活动相溶剂应具有低粘度、与检测器兼容性好、易于得到纯品和低毒性等特征。

挑选活动相时应考虑以下几个方面：

①活动相应不改动填料的任何性质。低交联度的离子交换树脂和排阻色谱填料有时遇到某些有机相会溶胀或缩短，然后改动色谱柱填床的性质。碱性活动相不能用于硅胶柱体系。酸性活动相不能用于氧化铝、氧化镁等吸附剂的柱体系。

②纯度。色谱柱的寿数与很多活动相经过有关，特别是当溶剂所含杂质在柱上堆集时。

③有必要与检测器匹配。运用UV检测器时，所用活动相在检测波长下应没有吸收，或吸收很小。当运用示差折光检测器时，应挑选折光系数与样品不同较大的溶剂作活动相，以进步灵敏度。

④粘度要低（应<2cp）。高粘度溶剂会影响溶质的分散、传质，下降柱效，还会使柱压降添加，使别离时刻延伸。最好挑选沸点在100℃以下的活动相。

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<section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 10px auto; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; text-align: center;"><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box; overflow-wrap: break-word !important; display: inline-block;"><section style="margin: 0px; padding: 1em; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; border-width: 8px; border-style: solid; border-color: rgb(235, 238, 237) rgb(235, 238, 237) rgb(235, 238, 237) rgb(207, 21, 18);"><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; text-align: justify; line-height: 1.75em; letter-spacing: 1.5px; font-size: 14px;"><p style="margin-top: 0px; margin-bottom: 0px; padding: 0px; outline: 0px; max-width: 100%; clear: both; min-height: 1em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-family: 微软雅黑; background-color: rgb(254, 254, 254); letter-spacing: 1px; color: rgb(0, 209, 0);">昨日的别离度不太行呀，活动相要再调调！”这话是不是很熟悉？调调？！咋调？假如你还不知道怎么制造适宜的活动相瞅这儿！</span></p></section></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; display: flex; justify-content: flex-start;"><section style="margin: -8px 0px 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; width: 236.938px; height: 8px; background: rgb(207, 21, 18);"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: -8px 0px 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; width: 0px; height: 1px; border-top: 8px solid rgb(207, 21, 18); border-right: 8px solid transparent;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section></section></section></section></section></section></section><p><br/></p><section data-support="96编辑器" data-style-id="26223" style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 10px 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; text-align: center; line-height: 1.75em;"><section style="margin: 0px; padding: 3px 25px; outline: 0px; max-width: 100%; box-sizing: border-box; overflow-wrap: break-word !important; border-width: 5px; border-style: solid; border-color: rgb(255, 191, 201); box-shadow: rgb(255, 49, 49) 0px 0px 5px inset; border-radius: 40px; display: inline-block; background-color: rgb(250, 132, 151);"><p style="margin-top: 0px; margin-bottom: 0px; padding: 0px; outline: 0px; max-width: 100%; clear: both; min-height: 1em; letter-spacing: 2px; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; color: rgb(255, 255, 255); font-size: 16px; letter-spacing: 1px;"><strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;">诀窍1：由强到弱</strong></span></p></section></section></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; letter-spacing: 1px;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px;">一般先用90%的乙腈(或甲醇)/水(或缓冲溶液)进行实验，这样能够很快地得到别离成果，然后依据出峰状况调整有机溶剂(乙腈或甲醇)的份额。 </span></span></section><section data-support="96编辑器" data-style-id="26223" style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 10px 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; text-align: center; line-height: 1.75em;"><section style="margin: 0px; padding: 3px 25px; outline: 0px; max-width: 100%; box-sizing: border-box; overflow-wrap: break-word !important; border-width: 5px; border-style: solid; border-color: rgb(255, 191, 201); box-shadow: rgb(255, 49, 49) 0px 0px 5px inset; border-radius: 40px; display: inline-block; background-color: rgb(250, 132, 151);"><p style="margin-top: 0px; margin-bottom: 0px; padding: 0px; outline: 0px; max-width: 100%; clear: both; min-height: 1em; letter-spacing: 2px; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 16px; color: rgb(255, 255, 255); letter-spacing: 1px;"><strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;">诀窍2：三倍规矩</strong></span></p></section></section></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; letter-spacing: 1px;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px;">每削减10%的有机溶剂(甲醇或乙腈)的量，保存因子约添加3倍，此为三倍规矩。这是一个聪明而又省力的方法。调整的过程中，留意调查各个峰的别离状况。 </span><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px;"></span></span></section><section data-support="96编辑器" data-style-id="26223" style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); box-sizing: border-box !important; overflow-wrap: break-word !important;"><section style="margin: 10px 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; text-align: center; line-height: 1.75em;"><section style="margin: 0px; padding: 3px 25px; outline: 0px; max-width: 100%; box-sizing: border-box; overflow-wrap: break-word !important; border-width: 5px; border-style: solid; border-color: rgb(255, 191, 201); box-shadow: rgb(255, 49, 49) 0px 0px 5px inset; border-radius: 40px; display: inline-block; background-color: rgb(250, 132, 151);"><p style="margin-top: 0px; margin-bottom: 0px; padding: 0px; outline: 0px; max-width: 100%; clear: both; min-height: 1em; letter-spacing: 2px; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 16px; color: rgb(255, 255, 255); letter-spacing: 1px;"><strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;">诀窍3：粗调转微调</strong></span></p></section></section></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-family: 微软雅黑, "Microsoft YaHei"; font-size: 14px; letter-spacing: 1px;">当别离到达必定程度，应将有机溶剂10%的改动量调整为5%，并据此规矩逐步下降调整率，直至各组分的别离状况不再改动。</span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; letter-spacing: 1px; color: rgb(0, 209, 0);"><strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px;">1．活动相的性质要求一个抱负的液相色谱活动相溶剂应具有低粘度、与检测器兼容性好、易于得到纯品和低毒性等特征。</span></strong></span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px;">挑选活动相时应考虑以下几个方面：</span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px;">①活动相应不改动填料的任何性质。低交联度的离子交换树脂和排阻色谱填料有时遇到某些有机相会溶胀或缩短，然后改动色谱柱填床的性质。</span><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px; color: rgb(0, 209, 0);"><strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;">碱性活动相不能用于硅胶柱体系。酸性活动相不能用于氧化铝、氧化镁等吸附剂的柱体系。</strong></span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px;">②纯度。色谱柱的寿数与很多活动相经过有关，特别是当溶剂所含杂质在柱上堆集时。</span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px;">③有必要与检测器匹配</span><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px; color: rgb(0, 209, 0);">。<strong style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;">运用UV检测器时，所用活动相在检测波长下应没有吸收，或吸收很小。当运用示差折光检测器时，应挑选折光系数与样品不同较大的溶剂作活动相，以进步灵敏度。</strong></span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><span style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important; font-size: 14px; letter-spacing: 1px;">④粘度要低（应<2cp）。高粘度溶剂会影响溶质的分散、传质，下降柱效，还会使柱压降添加，使别离时刻延伸。最好挑选沸点在100℃以下的活动相。</span></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-spacing: 0.544px; text-align: justify; white-space: normal; background-color: rgb(255, 255, 255); line-height: 1.75em; box-sizing: border-box !important; overflow-wrap: break-word !important;"><br style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; box-sizing: border-box !important; overflow-wrap: break-word !important;"/></section><section style="margin: 0px; padding: 0px; outline: 0px; max-width: 100%; color: rgb(51, 51, 51); font-family: -apple-system, BlinkMacSystemFont, "Helvetica Neue", "PingFang SC", "Hiragino Sans GB", "Microsoft YaHei UI", "Microsoft YaHei", Arial, sans-serif; font-size: 17px; letter-sp

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