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62 6 3· 64 6 5 Fluorocarbon-1l3,(I,I,2-tnchloro-l,2,2-tnfluroethane), b p 48°C Sodmm sulfate, anhydrous crystal Sdlca gel, 60-200 mesh, Davidson Grade 950 or eqmvalent Should contam 1-2% water as defined by residue test at 130°C Adjust by overmght eqmlIbratlOn Ifneeded CalIbratIOn mixtures 65 1 Reference 011 PIpet 150 ml n-hexadecane, 150 ml Isooctane, and 10 0 ml chlorobenzene mto a 50 ml glass stoppered bottle Mamtam the mtegnty of the mixture by keepmg stoppered except when withdrawmg alIquots 652 Stock standard PIpet 10 ml reference 011 (6 5 1) mto a tared 200 ml volumetnc flask and Immediately stopper WeIgh and dilute to volume WIth fluorocarbon-I 13 653 Workmg standards Pipet appropnate volumes ofstock standard (652) mto 100 ml volum,etnc flasks accordmg to the cell pathlength to be used DIlute to volume WIth fluorocarbon-113 Calculate concentratIOn of standards from the stock standard 7 Procedure 71 72 73 7 4 7.5 76 77 Mark the sample bottle at the water memscus for later determmatlOn of sample volume If the sample was not aCidified at tIme of collectIOn, add 5 ml hydrochlonc aCId (6 1) to thesamplebottle Aftermlxmgthesample,checkthepHbytouchmgpH-senSitivepaper to the cap to msure that,the pH IS 2 or lower Add more aCId Ifnecessary Pour the sample mto a separatory funnel Add 30 ml fluorocarbon-l13 (62) to the sample bottle and rotate the bottle to nnse the Sides Transfer the solvent mto the separatory funnel Extract by shakmg vIgorously for 2 minutes Allowthelayerstoseparate Ftlter the solvent layer through a funnel contammg solvent-mOIstened filter paper mto a 100 ml volumetnc flask NOTE 1 An emulSIon that fads to dISSIpate can be broken by pourmg about I g sodmm sulfate (6 3) mto the filter paper cone and slowly drammg the emulSIOn through the salt Additional 1 g portIons can be added to the cone as reqmred Repeat (73 and 74) tWice more WIth 30 ml portIons of fresh solvent, combmlng all solvent mto the volumetnc flask Rinse the tIp of the separatory funnel, filter paper, and the funnel WIth a total of 5-10 ml solventandcollectthennsmgsmtheflask DIlutetheextractto100ml IftheextractIS known to contam greater than 100 mg of non-hydrocarbon orgamc matenal, pipet an appropnate portIon of the sample to a 100 ml volumetnc and dilute to volume Discard about 5-10 ml solutIOn from the volumetnc flask Add 3 g SIlIca gel (6 4) and a stlrrmg bar, stopper the volu~etncflask, and stIr the solutIOn for a mmlmum of 5 mm on a magnetIc stIrrer 418 1-2 I 11111111 II 111111111 I 1111PDF Image | Methods for Chemical Analysis of Water and Wastes
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