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6 Reagents 7. Procedure 6I 62 6 3 6 4 HydrochloncaCId, I I MIXequalvolumesofconc HClanddIstilledwater Fluorocarbon-113,(1,1,2-tnchloro-l,2,2-tnfluoroethane),b p 48°C SodlUm sulfate, anhydrous crystal CahbratiOn mIxtures 641 Reference Oil PIpet 150 ml n-hexadecane, 150 ml Isooctane, and 100 ml chlorobenzene mto a 50 ml glass stoppered bottle 'Mamtam the 'mtegnty of the mIxture by keepmg stoppered except when withdrawmg ahquots 642 Stock standard PIpet 1 0 ml reference Oil (6 41) mto a tared 200 ml volumetnc flask and ImmedIately stopper WeIgh and dl1ute to volume wIth fluorocarbon-113 643 Workmg standards PIpet appropnate volumes ofstock standard (6 4 2) mto 100 ml volumetnc flasks accordmg to the cell pathlength to be used Dl1ute to volume wIth fluorocarbon-113 Calculate concentratiOn of standards from the stock standard 7 1 7 2 7.3 74 75 76 7 7 78 Mark the sample bottle at the water memscus for later determmatiOn of sample volume If the sample was not aCImfied at time of collectiOn, add 5 ml hydrochlonc aCId (6 1) to thesamplebottle AftermlXlngthesample,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-113 (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 mmutes Allowthelayerstoseparate FIlter the solvent layer mto a 100 ml volumetnc flask through a funnel contammg solvent-m01stened filter paper NOTE: An emulsiOn that falls to dIssIpate can be broken by pounng about 1g sodlUm sulfate (6 3) mto the filter paper cone and slowly drammg the emulSIon through the salt AddItional 1g portiOns can be added to the cone as reqUIred Repeat (73 and 74) tWIce more WIth 30 ml portIons of fresh solvent, combmmg all solvent m the volumetnc flask Rmse the tIp of the separatory funnel, filter paper, and the funnel WIth a total of 5-10 ml fluorocarbon-113 and collect the nnsmgs m the flask DIlute the extract to 100 ml, and stopper the flask ' Select appropnate workmg standards and cell pathlength accordmg to the followmg table of apprOXImate workmg ranges Pathlength 10 mm 50 mm 100 mm Range 2-40 mg 04-8 mg 01-4 mg Scan standards and samples from 3200 cm-1 to 2700 cm-1 WIth fluorocarbon-113 m the reference beam and record the results on absorbance paper The absorbances of samples 413 2-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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