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56 57 58 59 Sulfunc ACId (1 4) Slowly add 200 ml H2S04 (sp gr 1 84) to 800 ml ofdIstIlled water PotaSSIUm bllodate (0 IN) DIssolve 3 249g potaSSIUm bllodate, preVIOusly dned 2 hours at103°C,IndIstIlledwateranddIluteto10lIters Storemaglassstopperedbottle PotaSSIUm bllodate (0 oo5N) DIlute 50 ml of0 IN potaSSIUm bllodate (57) to l-hter m a volumetncflask Storemaglassstopperedbottle StandardIzatIon of 0 00564N phenylarsme OXIde DIssolve approXImately 2g (± 19) KI (52) In 100 to 150 ml dIstIlled water, add 10 ml H2S04 SolutIon (56) followed by 20 ml ooo5N potaSSIUm bllodate solutIOn (5 8) Place In dark for 5 mInutes, dIlute to 300 ml and tItrate WIth 0 oo564N phenylarsme OXIde SolutIon (5 1) to a pale straw color Add a small scoop ofIndtcator (54) Walt untIl homogeneous blue color develops and contmue the titration drop by drop untIl the color disappears Run m duplIcate DuplIcate determmattonsshouldagreewlthm ±O05ml NPAO- 20x0005 - mlP AO Adjust P AO solutIon Ifnecessary and recheck 6, Procedure 61 Place 200 ml of sample In the sample contamer ThiS volume IS convement because the buret readIng In millIlIters IS eqmvalent to mg/1 CI Up to 2 mg/1ls relIably titrated thiS way SmallersamplealIquotsdIlutedto200mlareusedforconcentratIOnsgreaterthan2 mg/1 The constructIOn of the cell and electrode component usually reqmre 200 ml of sample 62 Place on electrode assembly 63 Add10mlKIsolutIOn(53) 64 Add1mlacetatebuffer(55) 65 TItrateWith0oo564NPAO(5 1) 66 As each mcrement IS added the needle deflects toward rest When the needle no longer deflects subtract the last drop added from the buret readmg to obtam the mg/l Cl Less and/or slower deflectIOn SIgnals that the end POInt IS near 7 calculatIOns 7.1 For 0 oo564N P AO and a 200 ml sample there are no calculatIOns The buret readIng IS In mg/l The last Increment, when the needle does not deflect toward rest, must be subtracted 8 PrecIsion and Accuracy 8 1 More than 20 laboratones analyzed prepared samples of 0 64 and 1'83 mg/1 total CI The relative standard deVIatIOns were 248% and 125% respectIvely and the relative errors were 85% and 88% respectively 3301-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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