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7 CalculatlOns where 8 ml = the number ofml ofP AO needed to tItrate the sample N =thenormahtyofthePAOusedtotItratethesample V = the volume ofsample taken (100 ml or a fractIon thereof) 21,150 was calculated from the number of eqUlvalents oflOdme produced when the potasslUm lOdlde was added and from the rearrangement of the equatlOn to produce the value m terms of mg/I PreclslOn and Accuracy 6 3 NOTE A 250 ml lodme flask would mcrease accuracy and preClSl0n by preventmg possIble loss of the lOdme generated upon addItion of potasslUm lOdlde and sulfunc aCId (63 1) 623 Add 15 ml sodlUm acetate solutlOn (5 5) 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 sodlUm formate solutlOn (56), mIX well Walt 5 mmutes 625 Purge the space above the sample WIth a gentle stream of mtrogen (57) for apprOXImately 30 seconds to remove bromme fumes 6 2 6 If a preCIpItate forms (Iron), add 0 5 g KP·2H20 (5 17) 6 2 7 A dIstIlled water blank must be run WIth each set of samples because of IodIde m reagents If a blank IS conSIstently shown to be zero for a partIcular "lot" of chemIcals It can then be Ignored TttratlOn 8 1 82 In a smgle laboratory (EMSL), usmg a mIxed domestIC and mdustnal waste effluent, at concentratlOns of 1 6, 4 1, 66, 11 6 and 21 6 mg/l of lOdlde, the standard devlatlOns were ±O 23, ±O 17, ±O 10, ±O 06 and ±O 50 mg/I, respectively In a smgle laboratory (EMSL), usmg a mlXed domestIC and mdustnal waste effluent at concentratIons of 41,66, 11 6 and 216 mg/I oflOdlde, recovenes were 80, 97, 97 and 92%, respectIvely 63 1 6 3 2 DIssolve approXImately 1g potasslUm lOdlde (5 4) m sample Add 10 ml ofH2S04 solutlOn (5 8) and place m dark for 5 mmutes TItrate WIth phenylarsme OXIde workmg standard (5 10) or sodlUm thlOsulfate workmg standard solutlOn (5 14) addmg mdlcator (5 11 or 5 15) as end pomt IS approached (hght straw color) TItrate to colorless solutlOn DIsregard returnmg blue color I-(mg/l) =21,150 ( ml~N) 345.1-3PDF Image | Methods for Chemical Analysis of Water and Wastes
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