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63 64 65 66 67 68 69 6 10 SulfuncaCId concentrated Starch solutlOn Prepare an emulslOn of 10 g soluble starch m a mortar or beaker wIth a small quantlty of dIstllled water Pour thIS emulslOn mto 1 hter ofbOllmg water, allow to boll a few mmutes, and let settle overmght Use the clear supernate ThIS solutlOn may be preserved by the additlOn of 5 ml per hter of chloroform and storage m a woe refngerator 64 1 Dry, powdered starch mdicators such as "thyodene" may be used m place ofstarch solutlOn PotassIUm fluonde solutlOn DIssolve 40 g KF82H20 m dIstl1led water and dl1ute to 100 ml SodIUm thlOsulfate, stock solutlOn, 075 N DIssolve 186 15 g Na2S20385H20 m bolled andcooleddIstIlledwateranddIluteto1hter Preservebyaddmg5mlchloroform SodIUm thlOsulfate standard tltrant, 00375 N Prepare by dllutmg 500 ml of stock solutlOn to 1 hter Preserve by addmg 5 ml of chloroform Standard sodIUm thlOsulfate, exactly 00375 N IS eqUIvalent to 0300 mg of DO per 1 00 ml StandardIze WIth 00375 N potassIUm bllodate PotassIUm bllodate standard, 0 0375 N For stock solutlOn, dIssolve 4873 g of potassIUm bllodate, prevlOusly dned 2 hours at 103°C, m 1000 ml of dIstilled water To prepare workmg standard, dllute 250 ml to 1000 ml for 00375 N bllodate solutlOn StandardizatlOnof00375NsodIUmthIosulfate DIssolveapprOXImately 2g(±109)KI m 100 to 150 ml dIstIlled water, add 10 ml of 10% H2S04 followed by 20 0 ml standard potaSSIUm bllodate (6 8) Place m dark for 5 mmutes, dl1ute to 300 ml, and tItrate WIth the standard sodIUm thlOsulfate (6 7) to a pale straw color Add 1-2 ml starch solutlOn and contmue the tltratlOn drop by drop untll the blue color dIsappears Run m duphcate DuphcatedetermmatlOnsshouldagreewithm ±O05ml As an alternatIve to the sodIUm thlOsulfate, phenylarsme OXIde (P AO) may be used ThIS IS avallable, already standardIzed, from commerCIal sources 7 Procedure 7I To the sample collected m the BOD mcubatlOn bottle, add 2 ml ofthe manganous sulfate solutlOn (6 1) followed by 2 ml of the alkahne lOdide-azide solutlOn (6 2), well below the surface of the hqUId, stopper WIth care to exclude aIr bubbles, and mIX well by mvertmg the bottle several tlmes When the preCIpItate settles, leavmg a clear supernatant above the manganese hydroxIde floc, shake agam When setthng has produced at least 200 ml of clear supernatant, carefully remove the stopper and Immediately add 2 ml of conc 1 H2S04 (6 3) (suifamic aCId packets, 3 g may be SubstItuted for H2SOS ) by allowmg the aCId to run down the neck of the bottle, re-stopper, and mIX by gentle mverSlOn untll the lOdme IS umformly dIstnbuted throughout the bottle Complete the analySIS withm 45 mmutes 72 Transfer the entIre bottle contents by mverSlOn mto a 500 ml WIde mouth flask and tItrate WIth 00375 N thlOsulfate solutlOn (6 7) (00375 N phenyarsme OXIde (P AO) may be substItuted as tItrant) to pale straw color Add 1-2 ml of starch solutlOn (6 4) or 01 g of powdered mdicator and contmue to tItrate to the first dIsappearance ofthe blue color 3602-3PDF Image | Methods for Chemical Analysis of Water and Wastes
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