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6. 7 Apparatus DigestlOn apparatus A Kjeldahl digestlOn apparatus wIth 800 or 100 ml flasks and suctIon takeoff to remove S03 fumes and water DisttllatIon apparatus The macro Kjeldahl flask IS connected to a condenser and an adaptor so that the dIstl1late can be collected MIcro Kjeldahl steam disttllatlOn apparatus IS commercIally aval1able disttlled water through an Ion exchange column contammg a strongly aCIdIc catton exchange resm miXed wIth a strongly basIc amon exchange resm RegeneratlOn of the column should be carned out accordmg to the manufacturer's mstructiOns NOTE 1: All solutlOns must be made WIth ammoma-free water 72 Mercunc sulfate solutIon DIssolve 8 g red mercunc oXIde (HgO) m 50 ml of 1 4 sulfunc aCId (10 0 ml conc H2S04 40 ml dIstl1led water) and dIlute to 100 ml wIth dIstl1led water 73 Sulfunc aCId-mercunc sulfate-potassIUm sulfate SolutIon DIssolve 267 g K2S04 m 1300 ml dIstl1led water and 400 ml conc H2S04 Add 50 ml mercunc sulfate SolutIon (7 2) and dilute to 2 hters wIth dlstl1led water 74 SodIUm hydroxIde-sodIUm thIosulfate solutton DIssolve 500 g NaOH and 25 g Na2S203-5H20 i l l dIst111ed water and dl1ute to 1 hter 75 MiXed mdicator MiX 2 volumes of 02% methyl red m 95% ethanol wIth 1 volume of o2% methylene blue m ethanol Prepare fresh every 30 days 76 Bonc aCId solutlOn DIssolve 20 g bonc aCId, H3B03, m water and dl1ute to 1 hter wIth dIstIlled water 77 Sulfunc aCId, standard solutiOn (0 02 N) 1 ml = 0 28 mg NH3-N Prepare a stock solutIon of approxImately 0 1 N aCId by dl1utmg 3 ml of conc H2S04 (sp gr 1 84) to 1 hter wIth CO2-free dIstilled water Dl1ute 200 ml of thIS solutlOn to 1 hter wIth CO2-free disttlled water StandardIze the approxImately 0 02 N aCId so prepared agamst 0 0200 N Na2C03solutIon ThIslastsolutiOnISpreparedbydissolvmg1060ganhydrousNa2C03, oven-dned at 1400C, and dl1utmg to 1 hter wIth CO2-free dIstl1led water NOTE2: An alternate and perhaps preferable method IS to standardIze the approxImately 0 1 N H2S04 SolutIon agamst a 0 100 N Na2C03 SolutIon By proper dl1utlOn the 0 02 N aCId can the be prepared 7.8 Ammomum chlonde, stock solutIon 10 ml = 10 mg NH3-N DIssolve 3819 g NH4CI In water and make up to 1 hter m a volumetnc flask wIth dIstIlled water 79 Ammomumchlonde,standardSolutIon 10ml=001mgNH3-N DIlute100mlofthe stock solutlOn (7 8) wIth dIstilled water to 1 hter m a volumetnc flask 710 Nessler reagent DIssolve 100 g ofmercunc lOdide and 70 g potaSSIUm lOdide m a small volume of dIstl1led water Add thIS mIxture slowly, wIth sttrnng; to a cooled SolutIon of 160 g of NaOH m 500 ml of dIstl1led water Dl1ute the mIxture to 1 hter The solutiOn IS stable for at least one year Ifstored m a pyrex bottle out ofdIrect sunlIght 6.1 6 2 Spectrophotometer for use at 400 to 425 nm wIth a hght path of 1 cm or longer 6 3 Reagents , 7.1 DIstl1ledwatershouldbefreeofammoma SuchwaterISbestpreparedbythepassageof 3513-2PDF Image | Methods for Chemical Analysis of Water and Wastes
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