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5. 6. Apparatus 5 1 ReductIOn column The column m FIgure I was constructed from a 100 ml pIpet by removmg the top portIon ThIS column may also be constructed from two pIeces of tubmgJomed end to end A 10 mm length of3 cm I D tubmg ISJomed to a 25 cm length of3 5mmI D tubmg 5 2 Spectrophotometer for use at 540 nm, provIdmg a lIght path of 1 cm or longer Reagents Granulated cadmIUm 40-60 mesh (MCB Reagents) Copper-CadmIUm The cadmIUm granules (new or used) are cleaned wIth dIlute HCl and coppenzed wIth 2% solutIOn ofcopper sulfate m the followmg manner 62 1 Wash the cadmIUm wIth dIlute HCl (6 10) and nnse wIth dlstIlled water The color ofthe cadmIUm should be sIlver 6 2 2 SWIrl 25 g cadmIUm m 100 ml portIOns of a 2% solutIOn of copper sulfate (6 11) for 5 mmutes or untIl blue color partIally fades, decant and repeat wIth fresh copper sulfate untIl a brown collOIdal preCIpItate forms 623 Wash the copper-cadmIUm WIth dIstIlled water (at least 10 tImes) to remove all the precIpItated copper The color of the cadmIUm so treated should be black PreparatIon ofreactIOn column Insert a glass wool plug mto the bottom ofthe reductIOn column and fill WIth dIstIlled water Add suffiCIent copper-cadmIUm granules to produce a column 18 5 cm m length Mamtam a level of dIstIlled water above the copper- cadmIum granules to elImmate entrapment ofaIr Wash the column WIth 200 ml ofdIlute ammOnIum chlonde solutIOn (65) The column IS then actIvated by passmg through the column 100 ml ofa solutlOn composed of25 m1 ofa 1 0 mg/l N03-N standard and 75 ml of ammOnIum chlonde - EDT A solutIOn (6 4) Use a flow rate between 7 and 10 ml per minute AmmOnIum chlonde - EDT A solutIon DIssolve 13 g ammOnIum chlonde and 1 7 g disodIUm ethyienediamme tetracetate m 900 ml of dIstIlled water Adjust the pH to 8 5 with cone ammOnIum hydroxIde (6 9) and dIlute to 1lIter DIlute ammOnIum chlonde-EDT A solutIOn DIlute 300 ml ,of ammonIUm chlonde- EDTA solutIOn (6 4) to 500 ml WIth dIstIlled water Color reagent DIssolve 10 g suifamiamide and 1 g N(l-naphthyl)-ethylene-diamme dlhydrochlonde m a mixture of 100 ml conc phosphonc aCid and 800 m1 of distIlled water and dIlute to 1 lIter With distilled water Zmc sulfate solution Dissolve 100 g ZnS04-7H20 m distIlled water and dIlute to 1 lIter Sodium hydroxide sohitIOn, 6N Dissolve 240 g NaOH m 500 ml distIlled water, cool and dIlute to 1 lIter and dIlute to 1 lIter 6 12 Stock mtrate solution Dissolve 7 218 g KN03 m distilled water and dIlute to 1000 ml Preserve With 2 ml of chloroform per lIter ThiS solutlOn IS stable for at least 6 months 6.1 6 2 63 6.4 65 66 67 68 AmmonIum hydroxide, conc 69 6 10 DIlute hydrochlonc aCid, 6N Dilute 50 JIll ofconc HCI to 100 ml WIth distIlled water 6 11 Copper sulfate solutlOn, 2% DIssolve 20 g of CuS04-5H20 m 500 ml of distIlled water 1 O m l = l 0 0 m g N 0 3- N I 3533-2 'PDF Image | Methods for Chemical Analysis of Water and Wastes
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