(精)样品准备_英文.pptVIP

CEE 772 #22 * SPE cont. Cut-away of a syringe barrel From: Solid Phase Extraction by Thurman Mills * CEE 772 #22 * Sample Preparation——Basics and Physical Methods Updated: * CEE 772 #22 * Pretreatments to LLE Acidify to 2 8040: Phenols No pH adjustment 8060: Phthalate Esters 8100: PAHs Neutralize 8080: Oganochlorine pesticides PCBs 8090: nitroaromatics cyclic ketones 8140: organophosphorus pesticides Alkaline (11) then acidify (2) 8250 8270: GC/MS for Semivolatiles Drying is sometimes necessary 10 cm column of anhydrous Na2SO4 Addition of powdered anhydrous MgSO4 CEE 772 #22 * Soxhlet Extraction Good for soils, sediments sludges Used with thimbles Or glass wool plugs Typical extraction solvents Toluene/methanol (10:1) Acetone/hexane (1:1) Methylene chloride CEE 772 #22 * Distillation Theory CEE 772 #22 * Kuderna Danish Concentrators Ideal for concentrating ether extracts Common procedures Use with heated water bath Boiling chips Good to pre-wet snyder column by adding 1 mL of solvent to top Balls should “chatter”, but chambers should not be flooded May take 10-20 minutes Stop at apparent volume of ~1 mL Exchange solvent may be added at this time concentration continued CEE 772 #22 * Rotary Evaporation Rotary evaporators (also called rotavaps in lab slang) are used to remove solvents from reaction mixtures and can accommodate volumes as large as 3 liters. A typical rotary evaporator has a heatable water bath to keep the solvent from freezing during the evaporation process. The solvent is removed under vacuum, is trapped by a condenser and is collected for easy reuse or disposal. Most labs use a simple water aspirator vacuum on their rotavaps, so a rotavap can not be used for air and water-sensitive materials unless special precautions are taken. CEE 772 #22 * Use of Rotavaps Empty and then replace the solvent collection flask on the unit. Place your flask on the rotary evaporator. Use the speed contro