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7. 62 Flurocarbon-1l3,(1,1,2-tnchloro-1,2,2-tnfluoroethane), b p 48°C 6 3 SodIUm sulfate, anhydrous crystal Procedure 7 1 Mark the sample bottle at the water memscus for later determInatlOn of sample volume If the sample was not aCIdIfied at time of collectlOn, add 5 ml hydrochlonc aCId (6 1) to the sample bottle Mter mIXIng the sample, check the pH by touchIng pH-sensItive paper to the cap to Insure that the pH IS 2 or lower Add more aCId Ifnecessary 7 2 Pour the sample Into a separatory funnel 73 TareabOIlIngflask(pre-dnedInanovenat103°CandstoredInadeSIccator) 8 74 75 76 7.7 78 7 9 CalculatIon 8.1 mg/1 total oIl and grease = R VB where R= reSIdue,grossweIghtofextractlOnflaskmInUSthetareweIght,InmIllIgrams B = blank determInatlOn, reSIdue of eqUIvalent volume of extractlOn solvent, III mIllIgrams V = volume of sample, determIned by reftllIng sample bottle to calIbratlOn lIne and correctIng for aCId addItIon If necessary, In lIters Add 30 ml fluorocarbon-113 (62) to the sample bottle and rotate the bottle to rInse the sIdes Transfer the solvent Into the separatory funnel Extract by shakIng vIgorously for 2 . mmutes Allow the layers to separate, and ftlter the solvent layer Into the flask through a funnel contaInIng solvent mOIstened ftlter paper NOTE: An emulslOn that faIls to dIssIpate can be broken by pounng about 1 g sodIUm sulfate (6 3) mto the ftlter paper cone and slowly draInIng the emulsIon through the salt AdditlOnal 1 g portlOns can be added to the cone as requIred Repeat (7 4) tWIce more, WIth additlOnal portlOns offresh solvent, combInIng all solvent In thebOIlIngflask RInse the tip ofthe separatory funnel, the ftlter paper, and then the funnel WIth a total of 10-20 ml solvent and collect the nnSIngs In the flask Connect the bOIlIng flask to the dIstIllIng head and evaporate the solvent by ImmerSIng the lower half of the flask In water at 70°C Collect the solvent for reuse A solvent blank should accompany each set ofsamples When the temperature In the dIstIllIng head reaches 50°C or the flask appears dry remove thedIStillInghead Sweepouttheflaskfor15secondsWIthaIrtoremovesolventvaporby InsertIng a glass tube connected to a vacuum source ImmedIately remove the flask from the heat source and WIpe the outsIde to remove excess mOIsture and fingerpnnts Cool the bOIlIng flask In a deSIccator for 30 mInutes and weIgh 413 1-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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