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NITROGEN, KJELDAHL, TOTAL Method 351.4 (Potentiometric, Ion Selective Electrode) STORET NO. 00625 1 Scope and ApplicatiOn 1 1 ThIS method IS applicable to the measurement of TKN III dnnklllg and surface water, domestIc and llldustnal wastes 1 2 ThIS method covers the range from 0 03 to 25 mg TKN/1 2 Summary of Method 2 1 FolloWlllg dIgestiOn and cooling, dlstl1led water IS added to the dIgestiOn flask and the pH adjusted to between 3 and 4 5 by the addItiOn of 10 N NaOH The sample IS cooled and transferred to a 100 ml beaker After lllsertlllgthe electrode llltO the sample, NaOH- NaI-EDTA IS added and the ammoma measured (Ethylene diamllle tetraacetIc aCId (EDTA) IS added to the alkaline reagent (NaOH-NaI) to prevent precIpItatiOn of hydroXIdes, thereby aVOldlllg deposItiOn on the electrode membrane) 3 Sample Handling and PreservatiOn 31 SamplesmaybepreservedbyaddItiOnof2mlofconc H2S04 perliterandstoredat4°C Even when preserved III thIS manner, converSiOn of orgamc mtrogen to ammoma may occur Preserved samples should be analyzed as soon as possIble 4 Interferences 4 1 Interference from metals IS elimlllated WIth the addItion ofNaI 42 HIgh mtrate concentratiOns (lOX or more than the TKN level) result III low TKN values The reactiOn between mtrate and ammoma can be prevented by the use of an amon exchange reSlll (chlonde form) to remove the mtrate pnor to the TKN analysIs 5 Apparatus 51 Electrometer (pH meter) wIth expanded mV scale 52 Ammoma selectIve electrode, such as Onon Model 95-10 53 MagnetIc stIrrer, thermally lllsulated and Teflon-coated stIrrlllgbar 54 DIgestiOn apparatus A Kjeldahl dIgestiOn apparatus wIth 800 or 100 m1 flasks and suction take off to remove S03 fumes and water 55 Techmcon Block Dlgestor BD-40 6 Reagents 61 6 2 Dlstl1led water should be free of ammoma Such water IS best prepared by passlllg dlstl1led water through an IOn exchange column contallllllg a strongly aCIdIC catIOn exchange reSlll mIxed wIth a strongly basIc amon exchange reSlll RegeneratIOn of the column should be carned out accordlllg to the manufacturer's lllstructl0ns NOTE 1: All solutiOns must be made wIth ammoma-free water Mercunc sulfate solutIOn DIssolve 8 g red mercunc oXIde (HgO) III 50 ml of 1 4 sulfunc aCId (10 0 m1 conc H2S04 40 ml dIstilled water) and dl1ute to 100 ml wIth dlstl1led water Pendmg approval for NPDES Issued 1978 3514-1 IPDF Image | Methods for Chemical Analysis of Water and Wastes
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