Stationary phases I固定相的我.pptVIP

Flash injector 200:1 Splitless injector Gas removals Liquids: contain dissolved gases Ultrasound: cheap Non effective Vacuum: Higher price effective Effect of gas bubbles: In pump: Pressure pulsation Different flow-rates Mechanical instability In detector: Increased noise (retention time changes) He-purge: Higher price effective Remove of gas from the solvent: Sample loading Quick Sample should be mixable with eluent Sample volume: 10-50 ?l Micro syringe: ?Six-port” valve Columns Function: separation Liquid chromatography: NP LC: Normal Phase RP LC: Reversed Phase NPLC: polarity of stationary phase polarity of mobile phase RPLC: polarity of stationary phase polarity of mobile phase Material of column: Stainless steel Glass PEEK (poly(ether-ether-ketone) Size of column: diameter: 2-5 mm length: 5-25 cm Packing: regular spherical Modified silica gel SiO2 OH OH OH OH OH Modifying groups: C18: octadecyl: C18H37 C8: octyl: C8H17 C4: buthyl: C4H9 Amino: CH2CH2CH2NH2 Ciano: CH2CH2CH2CN Phenyl: C6H5 Guard column: avoid contamination of analytical column RPLC: C18 stationary phase methanol/water mobile phase NPLC: silicagel stationary phase hexane/alcohol mobile phase Detectors Quantitative analysis: signal of detector is proportional with concentration of analytes in detector universal: signal for every compounds selective: signal for a groups of compounds specific: signal for special compounds destruktiv non destruktiv Dinamic range: change of concentration results a change in signal linearity: T= mc (deviation 5 %) sensitivity: m (ratio of signal/concentration) Limit of detection (LOD): signal to noise ratio: 3 Limit of quantitation (LOQ): signal to noise ratio: 10 * Chromatographs eluent tank pump injector column detector PC CHROMATOGRAM Qualitative Quantitative information GasChromatography (GC) 1952: A.T. James A.J.P. Martin MOBILE PHASE: GAS STATIONARY PHASE: solid or liquid on solid support (GSC, GLC) COLUMN ELUTION TECHNIQUE GASCHROMATOGRAP