色譜柱和色譜系統(tǒng)的故障檢修ppt34-經(jīng)營(yíng)管理-展示頁
2024-08-26 17:39本頁面
【正文】 ? 50% 甲醇 : 50% 氯仿 ? 100% Ethyl Acetate 乙酸乙酯 2020/9/18 8 How to Change a Frit 怎樣更換濾頭 ? Column Inlet Frit 柱進(jìn)口濾頭 ? Column Body 柱身 ? Compression Ferrule 壓縮金屬套圈 ? Wear gloves 戴手套 ? Do not allow bed to dry 不要讓底座干燥 ? Do not touch the columnbody heat will extrude packing 不要使柱身受熱 ,否則填料會(huì)噴出 ? Do not over tighten 不要旋得太緊 ? Female End Fitting 旋好尾端螺母 ? Male End Fitting 旋好尾端螺頭 2020/9/18 9 Preventing Back Pressure Problems 壓力問題的預(yù)防 ? Use column protection 柱保護(hù) ? Guard columns 保護(hù)柱 /預(yù)柱 ? Inline filters 在線過濾器 ? Sample Preparation 樣品預(yù)處理 ? Appropriate column flushing ? 適當(dāng)?shù)闹鶝_洗 ? Filter buffered mobile phase ? 過濾緩沖流動(dòng)相 2020/9/18 10 Preventing Back Pressure Problems:InLine Devices 壓力問題的預(yù)防 :在線裝置 ? Mobile Phase PreColumn Injector Filter Guard ? From Pump 預(yù)柱 進(jìn)樣器 濾頭 Column ? 從泵來的流動(dòng)相 保護(hù)柱 ? Analytical ? Column ? Filter and Guard Column Act on Sample 分析柱 ? 濾頭和保護(hù)柱作用于樣品 ? PreColumn Acts on Mobile Phase ? 預(yù)柱作用于流動(dòng)相 To Detector ? 到檢測(cè)器 2020/9/18 11 Preventing Back Pressure Problems: Sample Preparation 壓力問題的預(yù)防 :樣品制備 ? Solvent/Chemical Environment ? 溶劑 /化學(xué)環(huán)境 ? Particulate/Aggregate Remove ? 微粒 /凝聚物的除去 ? Filter samples 過濾樣品 ? Centrifugation 離心分離 ? Solid Phase Extraction(.) 固相萃取 ? Cartridges or Plates 薄膜或薄層板 ? Disks or Membranes 圓盤或生物膜 2020/9/18 12 Peak Shape Issues 峰形問題 ? Split peaks 裂峰 ? Peak tailing 峰拖尾 ? Broad peaks 寬峰 ? Poor efficiency 低柱效 ? Many peak shape issues also . Broad and tailing or tailing with increased retention許多峰形問題是結(jié)合在一起的 例如 : ? 展寬和拖尾或拖尾和保留時(shí)間增加 2020/9/18 13 Split Peaks 裂峰 ?Can be caused by: ?可能的原因 : ? Column contamination 柱污染 ? Partially plugged frit 部分阻塞濾片 ? Column void 柱頭塌陷 ? Injection solvent effects 溶劑效應(yīng) 2020/9/18 14 Split Peaks 裂峰 Column Contamination 柱污染 ? Column: StableBond SBC8, 250mm, 5181。C ? Detection: UV 254 nm ? Sample: Filtered OTC Cold Medication: ? 1. Pseudoephedrine 2. APAP 3. Unknown ? 4. Chlorpheniramine ? Injection 1 峰 3 峰形較好 ? Injection 30 峰 3 裂峰 ? Injection 1 After Column Wash with 100% CAN ? 經(jīng) 100%乙腈沖洗后 峰 3 峰形極好 2020/9/18 15 Split Peaks 裂峰 Injection Solvent Effects 溶劑化效應(yīng) ? Column: StableBond SBC8, 250mm, 5181。L ? Sample: ? 1. Caffeine 咖啡因 2. Salicylamide 水楊酰胺 ? A. Injection Solvent B. Injection Solvent ? 100% Acetonitrile Mobile Phase ? 峰形寬拖尾 峰形尖銳對(duì)稱 ?樣品溶劑盡可能與流動(dòng)相匹配 2020/9/18 16 Determining the Cause of Split Peaks 裂峰原因的確定 ? 1. Complex sample matrix or many samples analyzed likely column contamination or partially plugged frit ? 復(fù)雜樣品的基質(zhì)或分析許多樣品 柱污染或部分阻塞濾片 ? 2. Mobile phase pH=7 likely column void due to silica dissolution (unless specialty column used) ? 流動(dòng)相 pH=
環(huán)評(píng)公示相關(guān)推薦
鄂ICP備17016276號(hào)-1