層析技術.pptVIP

吹氣捕捉裝置 層析管柱之種類Column Types LENGTH (meters) I.D. (mm) .5-10 2-4 5-100 .530 5-100 .1-.25 PACKED SERIES 530 NARROW BORE 填充管柱 Packed 毛細管柱 Open (Capillary) Wall Coated Open Tube 管柱-填充管柱 玻璃管柱 長 1.5至 3 m 內徑 2至 4 mm 內部填充表面被覆一層液相的小固體顆粒( 60至100篩目的矽藻土或碳化物) 管柱-毛細管柱 開口式玻璃毛細管柱 長 15至 100 m 內徑 0.2至 0.75 mm 管柱裡面塗敷一層液相，現在大部分的毛細管柱是使用熔矽材質，而玻璃管柱也仍被用來分析揮發性有機物 毛細管柱的分離效果比填充管柱好 10% of Applications Carrier Gas Adsorbent Packed Columns Adsorbent Packing (GSC) Capillary - Porous Layer Open Tubular (PLOT) Porous with large surface area Carrier Gas Gas Solid Chromatography (GSC) Partition Packing Packed Columns Carrier Gas Liquid Phase Solid Support Very porous with very high surface area Gas Liquid Chromatography (GLC) Wall Coated Open Tubular (WCOT) Liquid Phase Capillary Columns (90% Of Applications) Like dissolves like or Polar interacts with polar Separation by partitioning or differential solubility in stationary phase Components are separated based on differences in polarity (interaction of dipole forces) Generally Example: Alcohols are polar Carbowax is polar liquid phase Gas Liquid Chromatography (GLC) Parameter effect on R down sides Column length the longer the better longer elution time Film thickness the thinner the better smaller sample loads poor retention for extremely volatile compounds Inner diameter the smaller the better smaller sample loads Summary of column parameters on Resolution 不同型式管柱性能之比較Comparison of Column Types Packed Column Analysis: Capillary Conventional 5% OV101 on 80/100 Chromosorb 30m X 0.53mm X .88m 30m X 0.32mm X .25m HP Column Evaluation Sample 理想偵檢器特性 適當靈敏度(Sensitivity) 穩定性(Stability)及再現性(Reproducibility)佳 適當線性範圍(Linear dynamic range) 適當溫度範圍 反應時間(Response time)短且不受載流氣體流速影響 內容積小以避免溶質帶變寬 對所有溶質都有類似訊號或對一或多種類型溶質具選擇性感應 對溶質沒有破壞性 高可信度且使用方便 熱傳導度偵檢器 Thermal Conductivity Detector (TCD) 火燄離子化偵檢器 Flame Ionization Detector (FID) 電子捕捉偵檢器 Electron Capture Detector (ECD) 氮磷偵檢器