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7 <br /> WOW <br /> h <br /> 7.4.3 Sonicate for 3 min, with output control knoll set at lid <br /> and with mode switch on Pulse and pe Probe' cycle <br /> knob set at 508. Do hDT use microtip <br /> No. 41. filter <br /> nan <br /> 7.4.4 Decant and f vlt n�sn�filtrationoonccentr'ifuge and decent <br /> paper using, <br /> extraction solvent. <br /> 7.4.5 Repeat the extracortionstwo <br /> ofor more solvent. times <br /> Decant the' <br /> additional 100-ml, p <br /> extraction solvent after enc`+ sonication. on the final <br /> sonication, pour the entire sample into the Buchner <br /> funnel and rinse with extraction solvent. <br /> 7.4.6 Assemble a Kuderna-Danish (K-D) concentrator by <br /> attaching a 10-mL concentrator tube to a 500-m1- <br /> evaporative flask. <br /> 7,1f,7 Dry the extract by passing it through a drying coluFr.n <br /> anhydrous sodium sulfate. <br /> containing about 10 cm of <br /> Collect the dried extract intrator• �'a <br /> n a K-D conce <br /> the extractor flask and sodium sulfate column with 100- <br /> 125 mL of extraction solvent to complete the' <br /> quantitative vransfer. <br /> 7,4.8 Add one or two clean boiling Chips to the evaporative <br /> flask and attach a three-ball Snyder column. Prewet. the <br /> Snyder column by adding about methylene <br /> chloterbath <br /> ridt <br /> to the top. Place the K-D apparatus on <br /> (80-909c) so that the concentrator tube is partiall} <br /> immersed in the t:ot water and the entire lower rounds <br /> surface of the flask is bathed with s vapor, <br /> r,athe nd <br /> the vertical position of Che app <br /> temperature, as required, to cc..plete the concentration <br /> in 10-15 min. At the proper rate of distillation the <br /> balls of the column will actively chatter, but the <br /> chambers will not flood with condensed solvent. When <br /> apparent volume of liquid reaches 1 mL, remove the <br /> the <br /> thend allow it to drain and cool for at <br /> apparatus a <br /> least 10 min. <br /> uired (as <br /> 7.4•9 if 1) asolvent momentarily hremoveange SthegSnyder column indicated add 50 ml. of <br /> lvent and a new boiling chip, and re <br /> the exchange soConcentrate the extract - <br /> attach the Snyder column. re <br /> described in Paragraph 7.4.8, raising the <br /> maintain temperature <br /> of the water 'cath, if necessary, <br /> distillation. <br /> 7.4,10 Remove the Snyder column and rinse the flask and its <br /> lower joints into the concentrator tube with 1-2 mL of <br /> methylene chloride or exchange Coolvent.Method 3b 0 forif lfur <br /> crystals are a problem, Proceed <br />