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6 Procedure 6 1 6 2 Pretreatment 6 1 1 Add a vIsIble excess of CaO (5 5) to 400 ml of sample StIr or shake vIgorously for approxImately 5 mmutes Fl1ter through a dry, moderately retentive filter paper, dlscardmg the first 75 ml Iodme DetermmatlOn 62 1 Place 100 ml ofpretreated sample (6 1) or a fractlOn thereofdIluted to that volume, mto a 150 ml beaker Add a Teflon-coated stirnng bar and place on a magnetic stIrrer Insert a pH electrode and adjust the pH to approxImately 7 or shghtly less by the dropwlse addItion ofH2S04 solutlOn (5 12) 6 3 623 Add 15 ml sodmm acetate solutlOn (5 8) and 5 ml acetIc aCId solutlOn (5 1) MIX well Add 40 ml bromme water solutlOn (5 2), mIX well Walt 5 mmutes 624 Add 2 ml sodmm formate solutlOn (5 10), mIX well Walt 5 mmutes 6 2 5 Purge space above sample wIth gentle stream ofmtrogen (521) for approxImately 30 seconds to remove bromme fumes 626 IfaprecIpItateforms(Iron),add05gKFo2H20 (522) 6 2 7 A dlst111ed water blank must be run wIth each set of samples because of IodIde m reagents If the blank IS consIstently shown to be zero for a partIcular "lot" of chemIcals, It can be Ignored 628 TItrateasdescnbedm64 BromIde Plus IodIde DetermmatlOn 63 1 Place 100 ml ofpretreated sample (6 1) or a fractlOn thereofdl1uted to that volume, m a 150 ml beaker Add 5 g NaCI and stir to d1ss01ve Neutrahze by dropwlse add1tlOn ofHCl SolutIon (5 6) as m (6 2 1) Transfer as m (6 2 2) 6 3 2 Add 20 ml of calcmm hypochlonte solutlOn (5 4) Add 1 ml of HCI solutlOn (5 6) and add approxImately 0 2 g calcmm carbonate (5 3) 6 3 3 Heat to bOllmg on a hot plate, mamtam bOlhng for 8 mmutes j 634 Remove from hot plate and carefully add 4 ml sodmm formate solutlOn (5 10) CautlOn TOO RAPID ADDITION MAY CAUSE FOAMING Wash down sIdes wIth dIstIlled water 6 3 5 Return to hot plate and mamtam bOlhng condItions for an additlOnal 8 mmutes OccaslOnally wash down sIdes wIth dIstIlled water If resIdue IS deposIted from bOlhng actlOn 6 3 6 Remove from hot plate Wash down sIdes and allow to cool 637 Ifa precIpItate forms (Iron), add 05 g KFe2H20 (522) 63 8 Add 3 drops sodmm molybdate solutlOn (5 11) 6 3 9 A dIstIlled water blank must be run wIth each set of samples because of lOdlde, Iodate, bromIde, and/or bromate m reagents 6 3 10 TItrate as descnbed m 6 4 6 2 2 Transfer the sample to a 250 ml wIdemouthed comcal flask Wash beaker wIth small amounts of dlst111ed water and add washmgs to the flask A 250 ml lOdme flask would mcrease accuracy and preclSlon by preventmg possIble loss of the Iodme generated upon additlOn ofpotassmm lOdide and sulfunc aCId (64 1) 320 1-3PDF Image | Methods for Chemical Analysis of Water and Wastes
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