色譜柱和色譜系統(tǒng)的故障檢修ppt34-經(jīng)營管理(參考版)
2024-08-18 17:39本頁面
【正文】 , ?, and tr for suspect peaks 對懷疑峰 K180。 ?使用有機(jī)揮發(fā)性酸時(shí)，流動(dòng)相應(yīng)新配。) 容量因子改變 ? Selectivity changes (?) 選擇性改變 2020/9/18 28 Changes in Retention Same Column, Over Time相同柱子上保留時(shí)間改變 ,超時(shí) ? May be cause by: 可能的原因 : ? Column aging 柱老化 ? Column contamination 柱污染 ? Insufficient equilibration 不夠平衡 ? Poor column/mobile phase bination 柱 /流動(dòng)相組成差 ? Change in mobile phase 改變流動(dòng)相 ? Change in flow rate 改變流速 ? other instrument issues 其他儀器問題 2020/9/18 29 Mobile phase Change Causes Change in Retention 流動(dòng)相改變引起保留時(shí)間改變 ? 60%MeOH:40% % TFA Fresh TFA Added to Mobile Phase ? Volatile TFA evaporated/degassed from mobile phase. 易揮發(fā)的三氟乙酸從流動(dòng)相中蒸發(fā) /揮發(fā)。l extracolumn volume 50 181。m ? Mobile Phase: 40% 10 mM TEA, pH 11 : 60% MeOH ? Flow Rate: mL/min Temperature: . Detection: UV 254 ? Sample: 1. Maleat 順丁烯二酸 2. Pseudeophedrine 偽麻黃堿 3. Chlorphenniramine 氯非尼拉明 ? Plates 理論板數(shù) ? 1. 5922 ? 2. 9879 ? 3. 779 “ Phantom” peak from first injection 前次進(jìn)樣未出完的峰 ? The extremely low plates are an indication of an extremely late eluting peak from the preceding run. ? 極低的理論板數(shù)表明這是一個(gè)前面進(jìn)樣極遲洗脫出來的峰 2020/9/18 24 Peak Tailing峰拖尾 Injector Seal Failure進(jìn)樣器密封性差 ? Column: BonusRP, 75mm, ? Mobile Phase: 30% H2O : 70% MeOH Flow Rate: mL/min Temperature: . Detection: UV 254 nm ? Sample: 1. Uracil 尿嘧啶 2. Phenol 苯酚 ? 3. N,NDimethylaniline N,N二甲苯胺 ? Plates TF Plates TF ? 理論板數(shù) 拖尾因子 理論板數(shù) 拖尾因子 ? 1. 2235 1. 3670 ? 2. 3491 2. 10457 ? 3. 5432 3. 10085 ? Before After replacing rotor seal and isolation seal ? 之前 轉(zhuǎn)動(dòng)桿和隔離密封墊檢修后 ? Overdue instrument maintenance can cause peak shape problems. ? 儀器保養(yǎng)超期可能引起峰形問題 /進(jìn)樣器劃痕 2020/9/18 25 Peak Tailing 峰拖尾 ExtraColumn Volume 柱外死體積效應(yīng) ? Column: StableBond SBC18, 30mm, ? Mobile Phase: 85% H2Owith % TFA : 15% CAN ? Flow Rate: mL/min Temperature: 35186。 2％三乙胺 (~pH 11) ? After 30 injections Initial 開始時(shí) ? 進(jìn)樣 30次后 ? Multiple peak shape changes can be caused by the same column problem. In the case a void resulted from silica dissolved at high pH. ? 多數(shù)峰形改變可能是同一柱問題引起的。m ? Mobile Phase:40%25mM Na2HPO4, : 60%ACN ? Flow Rate: mL/min Temperature: 40186。m ? Mobile Phase: 20% H2O : 80% MeOH Flow Rate: mL/min Temperature: . Detection: UV 254 nm ? Sample: 1. Uracil 尿嘧啶 2. Phenol 苯酚 ? 3. 4Chloronitrobenzene 4氯硝基苯 4. Toluene 甲苯 ? Plates TF Plates TF Plates TF ? 理論板數(shù) 拖尾因子 理論板數(shù) 拖尾因子 理論板數(shù) 拖尾因子 ? 1. 7629 1. 7906 1. 7448 ? 2. 12043 2. 12
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