SIST EN 12260:2003
(Main)Water quality - Determination of nitrogen - Determination of bound nitrogen (TNb), following oxidation to nitrogen oxides
Water quality - Determination of nitrogen - Determination of bound nitrogen (TNb), following oxidation to nitrogen oxides
This European Standard specifies a method for the determination of nitrogen in water in the form of free ammonia, ammonium, nitrite, nitrate and organic compounds capable of conversion to nitrogen oxides under the oxidative conditions described. Determination is carried out instrumentally. Dissolved nitrogen gas is not determined by this method.
This method is applicable to the analysis of surface water, waste water and treated sewage effluent.
Wasserbeschaffenheit - Bestimmung von Stickstoff - Bestimmung von gebundenem Stickstoff (TNb) nach Oxidation zu Stickstoffoxiden
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Stickstoff in Wasser, gebunden als freier Ammoniak, Ammonium, Nitrit, Nitrat und organische Verbindungen fest, die unter den beschriebenen oxidativen Bedingungen zu Stickstoffoxiden überführt werden. Die Bestimmung wird instrumentell durchgeführt. Gelöster elementarer Stickstoff wird nach diesem Verfahren nicht erfasst.
Das Verfahren ist anwendbar auf die Untersuchung von Oberflächenwasser, Abwasser und Kläranlagenabläufen.
1.1 Anwendungsbereich des Bestimmungsverfahrens
Der Anwendungsbereich des Bestimmungsverfahrens hängt von dem gerätespezifischen Injektionsvolumen ab. Stickstoffmassenkonzentrationen von 1 mg/l bis zu 200 mg/l können bestimmt werden. Höhere Konzentrationen können, wenn nötig, nach Verdünnung der Wasserprobe bestimmt werden.
1.2 Bestimmungsgrenze
Die Bestimmungsgrenze hängt vom gerätespezifischen Injektionsvolumen ab. Beim Einsatz eines geeigneten Injektionsvolumens beträgt die Bestimmungsgrenze etwa 0,5 mg/l.
1.3 Störungen
In Abhängigkeit vom eingesetzten Gerät können Störungen durch Memoryeffekte eintreten. Diese können entweder durch Wasserproben oder durch Standardlösungen mit hohen Massenkonzentrationen an gebundenem Stickstoff verursacht werden.
ANMERKUNG Gegebenenfalls können Störungen auftreten, wenn die Wasserprobe einen hohen Gesamtgehalt an gebun-de-nem Kohlenstoff (TOC) aufweist. In diesem Fall können Minderbefunde auftreten. Etwaige Probleme können erkannt werden, indem der Stickstoff vor und nach Verdünnung der Probe bestimmt wird oder Standard-Additionsverfahren eingesetzt werden.
Nicht alle organischen Stickstoffverbindungen werden durch das beschriebene Verfahren quantitativ in Stickstoffoxide überführt (siehe Wiederfindungsraten in Tabelle B.1).
Qualité de l'eau - Dosage de l'azote - Dosage de l'azote lié (TNb) apres oxydation en oxydes d'azote
La présente Norme Européenne fixe une méthode de dosage de l'azote présent dans l'eau sous forme de gaz ammoniac libre, d'ammonium, de nitrite, de nitrate et de composés organiques capables de se transformer en oxydes d'azote sous l'effet des conditions oxydantes décrites. Le dosage est réalisé par une technique instrumentale. L'azote gazeux dissous n'est pas dosé par cette méthode.
Cette méthode s'applique a l'analyse des eaux de surface, des eaux résiduaires et des effluents d'eaux usées traitées.
La gamme de concentration de la méthode dépend du volume d'injection utilisé, lui-meme fonction de l'instrument utilisé. L'azote total peut etre dosé dans la plage de 1 mg/l a 200 mg/l. Des concentrations plus élevées peuvent, si nécessaire, etre déterminées par dilution de l'échantillon. La limite de détection dépend de l'instrument utilisé. Avec un volume d'injection approprié, la limite de détection est généralement d'environ 0,5 mg/l.
Kakovost vode – Določevanje dušika – Določevanje vezanega dušika (TNb) po oksidaciji do dušikovih oksidov
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Wasserbeschaffenheit - Bestimmung von Stickstoff - Bestimmung von gebundenem Stickstoff (TNb) nach Oxidation zu StickstoffoxidenQualité de l'eau - Dosage de l'azote - Dosage de l'azote lié (TNb) apres oxydation en oxydes d'azoteWater quality - Determination of nitrogen - Determination of bound nitrogen (TNb), following oxidation to nitrogen oxides13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN 12260:2003SIST EN 12260:2003en01-december-2003SIST EN 12260:2003SLOVENSKI
STANDARD
SIST EN 12260:2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12260September 2003ICS 13.060.50Supersedes ENV 12260:1996English versionWater quality - Determination of nitrogen - Determination ofbound nitrogen (TNb), following oxidation to nitrogen oxidesQualité de l'eau - Dosage de l'azote - Dosage de l'azote lié(TNb) après oxydation en oxydes d'azoteWasserbeschaffenheit - Bestimmung von Stickstoff -Bestimmung von gebundenem Stickstoff (TNb) nachOxidation zu StickstoffoxidenThis European Standard was approved by CEN on 1 August 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 12260:2003 ESIST EN 12260:2003
EN 12260:2003 (E)2ContentspageForeword.3Introduction.41Scope.52Normative references.53Principle.54Interferences.55Reagents.66Apparatus.67Sampling and sample preparation.78Procedure.79Establishment of the calibration curve.710System check.811Calculation.812Expression of results.813Test report.914Precision data.9Annex A (informative)
Determination of bound nitrogen using other techniques.10Annex B (informative)
Recovery rates of single compounds using oxidation andchemiluminescence detection (see table B.1).11Annex C (informative)
Precision data.12Bibliography.13SIST EN 12260:2003
EN 12260:2003 (E)3ForewordThis document (EN 12260:2003) has been prepared by Technical Committee CEN/TC 230 “Water analysis”,the secretariat of which is held by DIN.This European Standard shall be given the status of a national standard, either by publication of an identicaltext or by endorsement, at the latest by March 2004, and conflicting national standards shall be withdrawn atthe latest by March 2004.This document supersedes ENV 12260: 1996Annexes A B, and C are informative annexes.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark,Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands,Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 12260:2003
EN 12260:2003 (E)4IntroductionWARNING — Persons using this standard should be familiar with normal laboratory practice. Thisstandard does not purport to address all of the safety problems, if any, associated with its use. It isthe responsibility of the user to establish appropriate safety and health practices and to ensurecompliance with any national regulatory conditions.It is absolutely essential that tests carried out according to this European Standard are carried out by suitablyqualified staff.This European Standard specifies a method for the determination of total bound nitrogen after oxidation ofinorganic and organic nitrogen compounds by combustion to nitrogen oxides. Quantification is carried out bychemiluminescence.The procedure referred to in the normative part is the reference method. Whilst staying within the scope of thisstandard, it is permissible to use such alternatives as given in annex A only, provided that their performance isequal to or better than that given in clause 13 and tables in annex B and C, when calculated using proceduresgiven in ISO 5725-2, and when the comparison of performance data between this European Standard and anyalternative technique is carried out using the procedures described in ISO 2854.All references to nitrogen concentrations are expressed in units of mg/l N, i.e. milligrams of nitrogen per litresolution.SIST EN 12260:2003
EN 12260:2003 (E)51 ScopeThis European Standard specifies a method for the determination of nitrogen in water in the form of freeammonia, ammonium, nitrite, nitrate and organic compounds capable of conversion to nitrogen oxides underthe oxidative conditions described. Determination is carried out instrumentally. Dissolved nitrogen gas is notdetermined by this method.This method is applicable to the analysis of surface water, waste water and treated sewage effluent.The concentration range of the method will depend on the injection volume used which is instrument specific.Total nitrogen can be determined in the range from 1 mg/l up to 200 mg/l. Higher concentrations can, ifnecessary, be determined by dilution of the sample. The limit of detection will depend on the instrument inuse. Using a suitable injection volume, the limit of detection is typically round about 0,5 mg/l.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications.These normative references are cited at the appropriate places in the text, and the publications are listedhereafter. For dated references, subsequent amendments to or revisions of any of these publications apply tothis European Standard only when incorporated in it by amendment or revision. For undated references thelatest edition of the publication referred to applies (including amendments).EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987).EN ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples(ISO 5667-3:1994).ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basicmethods for the determination of repeatability and reproducibility of a standard measurement method.ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performancecharacteristics — Part 1 : Statistical evaluation of the linear calibration function.ISO 8466-2, Water quality — Calibration and evaluation of analytical methods and estimation of performancecharacteristics — Part 2: Calibration strategy for non-linear second order calibration function.3 PrincipleOxidation of the sample containing nitrogen by catalytic combustion in an oxygen atmosphere at > 700 °C, tonitrogen oxides. Quantification of nitrogen concentration is carried out by chemiluminescence detection (afterreaction with ozone).4 InterferencesDepending on the instrument in use, interferences may arise from memory effects. These may occur eitherfrom samples or standard solutions with high amounts of bound nitrogen.NOTEPotential problems can arise with samples containing significant total organic carbon (TOC) concentrations.The analysis of samples containing large amounts of TOC will lead to the reporting of lower results for nitrogen. Suspectedproblems can be identified by determining nitrogen before and after suitable dilution, or by using standard additiontechniques.Not all organic nitrogen compounds are qu
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