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107281993 141 303 490 1522 ATI FT COLLINS - � P.Op r <br /> 6.2 Fluorocarbon•113,(I.1.2.irichloroo-1,2,2-trinuroctliane).bp.48'C. <br /> 6.3 Sodium Sulfate,anhydrous crystal <br /> 64 Silks gal.6 200 meth. Davidson Grade 9SOor equivalent Should contain 1-21P water <br /> as defined by ttisidue test at I30'C.Adjust by overnight equilibration if nesdcd <br /> 6.5 Calibration mixtures <br /> ' 6 S 1 Reference oil Pipet 150 ml n-hcnadiecane. 15.0 ml luxictane, and 100 ml <br /> chlorobenzene into a SO ml glass stoppered bottle, Maintain the sntegrit1 of the <br /> mixture by keepin6 sitoppered incept when withdraw ins aliquot. <br /> 6.52 Stink standard: Pipet 10 ml reference oil(6 3 1) into a tared 200 ml %olumetri. <br /> flask and Immediately stopper.Weigh and dilute to volume with fiuorocartma.I I s <br /> 6J.3 Working>atindards Pipet al+propnatevolumesotstock standard(6 3 2)into 100 <br /> ml solumeiric flasks according to the cell pathleasth to be used Dilute to velums <br /> with Miarocarbon-113 Calculate concentration of standards from the %imk <br /> standard <br /> 7. Procedure <br /> ` 7 I Marie the sample bottle at the water meniscus for later determination of sample%ulumu <br /> If the%atriple was not acidified at time of collection.add S sol hydrochloric acid (6 I) to <br /> • the sample bottle After mixing the sample,check the pH by tauehing pH-senjitt+e par+-r <br />' lathe cap to insure that the rH 1-12 or lower Add more acid if netiensary <br /> 7 2 Pour the sample into,a scparatory funnel. <br /> 7.3 ' Add 30 ml fluorocarbon-10(6 2)to the sample bottle and total:. the bottle to nese the <br /> ' sides Transifer the solvent Into the separatory funnel.Extract by A)akinS vigorously for 2 <br /> Min utm Allow the layers Io vrwaic. <br /> 1 + 7 4 Filter the solvent layer through a funnel containing solvent-moistened filter parvr into a <br /> 100 ml volumetric Raek <br /> NOTE 1 An emulsion that fails to dissipate can be broken by pouring about I g%odsuns <br /> sulfate(6.3)Into the filter paper cone and slowly draining the emulsion through the silt <br /> Additional I g portions can be added to the cone as required. <br /> 7.5 Repeat (7.3 and 74) twice more with 3O m1 poptions of fresh Solvent, combining ,ill <br /> solvent Into the volumetric flask. <br /> 7.6 R:rise the tip of the separatory funnel.filter paper.and the funnel with a total of 3-10 mi <br /> ' <br /> SOY"[[and COW the ttimtrip in the flask. ptlute the extract in 100 ml If the cstract I% <br /> known to contain greater than I00 mg of non-hydrocarbon organic material pipet in <br /> cpprnprt_te portion of the sample tea 100 rill vo'umetnc and dilite to vc?urrse <br /> 7 7 Vi.eard ahout 5-10 till %glutton from the+olunoetne flask. Add 3 g silica gel (6 4) and 2 <br /> stirring haw,Vopper the volumetric Ila<k.and%tir the vtolution for a minimum of S min on <br /> a magnet ic stirrer. <br /> �r <br />