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Methods for Chemical Analysis of Water and Wastes

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Methods for Chemical Analysis of Water and Wastes ( methods-chemical-analysis-water-and-wastes )

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CYANIDES, AMENABLE TO CHLORINATION Method 335.1 (Titrimetric; Spectrophotometric) STORET NO. 00722 1 Scope and ApplicatlOn 11 ThIS method IS applIcable to the determmatlOn of cyamdes amenable to chlormatlOn m dnnkmg, surface and salIne waters, domestIc and mdustnal wastes 12 The titratlOn procedure IS used for measurmg concentratlOns of cyamde exceedIng 1 mg/l after removal of the cyamdes amenable to chlormatlOn Below th1s level the colonmetnc determmatlOn IS used 2 Summary of Method 2 1 A portlOn of the sample IS chlonnated at a pH> 11 to decompose the cyamde CyanIde levels m the chlonnated !>ample are then determmed by the method for Cyamde, Total, m thISmanual CyamdesamenabletochlormatlOnarethencalculatedbydIfference 3 Reagents 31 CalcIUm Hypochlonte SolutIon DIssolve 5 g of calcIUm hypochlonte (Ca(OC1)2) In 100 ml of dIstIlled water 32 SodIUm HydroxIde SolutIon DIssolve 50 g of sodIUm hydroxIde (NaOH) m dIstIlled water and dIlute to 1 liter 33 AscorbIc aCId crystals 34 PotassIUm IodIde-starch test paper 4 Procedure 41 Two sample alIquots are reqUIred to determme cyamdes amenable to chlormatlOn To one 500 ml alIquot or a volume dIluted to 500 ml, add calcIUm hypochlonte solutlOn (3 1) dropwise whIle agItatIng and mamtammg the pH between 11 and 12 WIth sodIUm hydroxIde (3 2) CautlOn The mitIal reactlOn product of alkaline chlonnatlOn IS the very tOXiC gas cyanogen chlonde, therefore, It IS recommended that thIS reaction be performed m a hood For convemence, the sample may be agItated m a l liter beaker by means of a magnetIc stIrnng deVIce 42 Test for reSIdual chlonne WIth KI-starch paper (34) and mamtam thIS excess for one hour, contmumg agitatlOn A dIstmct blue color on the test paper mdicates a suffiCIent chlonne level Ifnecessary, add additlOnal hypochlonte solutlOn 43 After one hour, add 05 g portlOns of ascorbIC aCId (3 3) until KI-starch paper shows no reSIdual chlonne Add an addItional 0 5 g ofascorbIc aCId to msure the presence ofexcess reducmg agent 44 Test for total cyamde m both the chlormated and unchlormated alIquots as In the method Cyamde, Total, m thIS manual Approved for NPDES Issued 1974 335 1-1

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