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7 63 Sulfunc aCId-mercunc sulfate-potassIUm sulfate solutIOn DIssolve 267 g K2S04 In 1300 ml dIstIlled water and 400 ml conc H2S04 Add 50 ml merCUrIC sulfate solutIOn (6 2) and dIlute to 2 lIters WIth dIstIlled water 6.4 SodIUm hydroxIde 10N DIssolve 400 g NaOH In 600 ml of ammoma-free water, cool and dIlute to 1lIter ' " 6.5 SodIUm HydroxIde, SodIUm IodIde and EDT A Solution DIssolve 400 g of NaOH, 300 g NaI and 2 g ofEDTA In 700 ml ofammoma-free water, cool and dIlute to 1lIter 66 Ammomum chlonde, stock solutIOn 10 ml = 10 mg NH3-N DIssolve 3819 g NH4CI m water and make up to 1 lIter In a volumetrIc flask WIth dIstIlled water 6.7 Ammomum chlorIde, standard solutIOn 10 ml = 001 mg NH3-N DIlute 10 0 ml of the stock solutIOn (6 6) to 1 lIter WIth dIStilled water In a volumetn:c flask Procedure 7.1 Macro KJeldahl system 72 73 MIcro KJeldahl system 721 Place 50 0 ml ofsample, or an ahquot dIluted to 50 ml, In a 100 ml KJeldahl flask and add 10 ml sulfUrIC aCId-merCUrIC sulfate-potassIUm sulfate solutIOn (63) Evaporate the mIxture In the KJeldahl apparatus untIl S03 fumes are gIven off and the SolutIon turns colorless or pale yellow Then dIgest for an addItional 30 mInutes CoolthereSIdue,add44mldIStilledwaterandmIX Block Digestor 7 3 1 Place 20 ml of sample, or an ahquot dIluted to 20 ml, In the dIgestIOn tube Add 5 77.1 Place a measured sample or the reSIdue from the dIstIllatIon In the ammoma determInatI,on (for Orgamc KJe1dahl only) Into an 800 ml KJeldahl flask The 7 3 2 733 mlofsulfUrICaCId-merCUrICsulfate-potasSIUmsulfatesolutIOn(63)andmIX Add 4-8 Teflon bOlhng stones Place tubes In wgestor that has been preheated to 200°C Set low temperature at 200°C for 1 hour, the hIgh temperature at 380°C and total time for two and one half hours sample SIze can be determmed from the follOWIng table ' , Kjedahl Nitrogen III Sample, mgll 0-5 5-10 10-20 20-50 50-500 Sample Size ml 500 250 100 500 250 DIlute the sample, If reqUIred, to 500 ml WIth dIstIlled water, and add 100 ml sulfUrIC aCId-merCUrIC sulfate-potassIUm sulfate solutIOn (63) and evaporate the mIxture In the KJeldahl apparatus untIl S03 fumes are' gIven off and the solution turnscolorlessorpaleyellow ContInueheatIngfor30addItionalmInutes Coolthe resIdue and add 500 ml dIstIlled water and mIX 3514-2 1 1111 11PDF Image | Methods for Chemical Analysis of Water and Wastes
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