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5 10 Phenylarsme OXIde Worlang Standard (00075 N) Transfer 100 ml of commerCIally avaIlable 00375 N phenylarsme OXIde (59) to a 500 ml volumetnc flask and dIlute to the markWIthdIstIlledwater ThISsolutIOnshouldbepreparedfreshdally 5 11 CommerCIally avaIlable starch mdicators such as thyodene or eqUIvalent may be used 5 12 513 5.14 5 15 5.16 5.17 518 SodIUm ThIOsulfate, Stock SolutIOn, 075 N DIssolve 186 15 g (Na2S203-5H20) m boiled and cooled dIstilled water and dIlute to 10 lIter Preserve by addmg 5 ml chloroform SodIUm ThIOsulfate Standard TItrant, 00375 N Prepare by dIlutmg 500 ml of stock SolutIon to 1 0 lIter Preserve by addmg 5 ml of chloroform StandardIze WIth 0 0375 N potasSIUm bllodate (5 15,5 18) SodIUm ThIosulfate Workmg Standard (00075 N) Transfer 100 ml of sodIUm thIOsulfate standard tItrant (5 13) to a 500 m1 volumetnc flask and dIlute to the mark WIth dIstI11ed water Tills solutIOn should be prepared fresh dally PotasSIUm Bllodate Standard, 00375 N DIssolve 4873 g potassIUm bllodate, preVIOusly dned 2 hours at 103°C, m dIstIlled water and dI1ute to 1 0 lIter DI1ute 250 ml to 1 0 lIter for 00375 N bllodate solutIOn Starch SolutIon Prepare an emulSIon of 10 g of soluble starch m a mortar or beaker WIth a small quantIty of dIstIlled water Pour thIS emulSIOn mto 1 lIter of bOIlIng water, allow to boll a few mmutes, and let settle overnIght Use the clear supernate ThIS SolutIon may be preserved by the addItIon of 5 ml per lIter of chloroform and storage m a 10°C refngerator CommerCIally avaIlable, powdered starch mdicators may be used m place ofstarch solutIOn PotasSIUm Fluonde (KP-2H20) ACS Reagent Grade StandardIzatIon of 00375 N Pheny1arsme OXIde and 00375 N sodIUm thIosulfate. DIssolve approxImately 2 g (± 109) KI (54) m 100 to 150 ml dIstIlled water, add 10 ml H2S04 solutIon (5 8) followed by 20 ml standard potaSSIUm bllodate solutIOn (5 15) Place m dark for 5 mmutes, dI1ute to 300 ml and tItrate WIth phenylarsme OXIde (5 9) or sodIUm thIOsulfate standard tItrant (5 13) to a pale straw color Add a small scoop ofmdIcator (5 11) Walt untIl homogeneous color develops and contmue the tItratIOn drop by drop untIl the blue color dIsappears Run m duplIcate DuplIcate determmations should agree Wlthm ±O 05 ml 6 Procedure 61 Pretreatment 6 1 1 Add a VISIble excess of CaO (5 3) to 400 ml of sample Stir or shake vIgorously for apprOXImately 5 mmutes PIlter through a dry, moderately retentIve filter paper, dlscardmg the first 75 ml 62 IodIde DetermmatIon 62 1 Place 100 ml ofpretreated sample (6 1) or a fractIOn thereofdI1uted 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 slIghtly less by the dropwise addItIOn ofH2S04 SolutIon (5 8) 622 Transfer the sample to a 250 ml WIde-mouthed corncal flask Wash beaker WIth small amounts ofdIstI11ed water and add washmgs to the flask 3451-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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