Sludge, treated biowaste and soil - Determination of Kjeldahl nitrogen

This European Standard specifies the determination of Kjeldahl nitrogen according to the Kjeldahl procedure in sludge, treated biowaste and soil. Nitrate and nitrite are not included. Compounds with nitrogen bound in N-N, N-O linkages and some heterocycles (pyridines) are only partially determined. The limit of detection (LOD) is usually 0,03 % nitrogen, and the limit of quantification (LOQ) is 0,1 % nitrogen (using 0,25 mol/l sulfuric acid for titration).

Schlamm, behandelter Bioabfall und Boden - Bestimmung des Kjeldahl-Stickstoffs

Diese Europäische Norm legt ein Verfahren zur Bestimmung des Stickstoffs nach Kjeldahl in Schlamm, behandeltem Bioabfall und Boden fest.
Der Stickstoff in Nitraten und Nitriten wird nicht erfasst.
Der in N N Verbindungen, N O Verbindungen sowie in einigen heterozyklischen Verbindungen (Pyridine) vorliegende Stickstoff wird nur teilweise erfasst.
Eine typische Nachweisgrenze (LOD, en: limit of detection) liegt bei 0,03 % Stickstoff und eine typische Bestimmungsgrenze (LOQ, en: limit of quantification) liegt bei 0,1 % Stickstoff (bei Verwendung von 0,25 mol/l Schwefelsäure für die Titration).

Boues, bio-déchets traités et sols - Détermination de l'azote Kjeldahl

La présente Norme européenne spécifie la détermination de l'azote Kjeldahl selon le mode opératoire de Kjeldahl, dans les boues, les biodéchets traités et les sols.
Les nitrates et les nitrites ne sont pas inclus.
Les composés comportant de l'azote lié dans des liaisons N-N, N-O et certains hétérocycles (pyridines) ne sont que partiellement déterminés.
La limite de détection (LD) est habituellement 0,03 % d'azote, et la limite de quantification (LQ) est 0,1 % d'azote (en utilisant l'acide sulfurique à 0,25 mol/l pour le titrage).

Blato, obdelani biološki odpadki in tla - Določevanje dušika po Kjeldahlu

Ta evropski standard opredeljuje določevanje dušika po Kjeldahlu v skladu s Kjeldahlovo metodo v blatu, obdelanih bioloških odpadkih in tleh. Nitrat in nitrit nista vključena. Spojine z dušikom, vezanim v N-N, N-O in nekaterih heterocikličnih spojinah (piridini) so samo delno določene. Meja detekcije (LOD) je običajno 0,03 % dušika, meja kvantifikacije (LOQ) pa je 0,1 % dušika (pri čemer se porabi 0,25 mol/l žveplove kisline za titracijo).

General Information

Status
Published
Public Enquiry End Date
19-Feb-2011
Publication Date
20-Jan-2013
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Jan-2013
Due Date
11-Mar-2013
Completion Date
21-Jan-2013

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.MHOGDKOXSchlamm, behandelter Bioabfall und Boden - Bestimmung des Kjeldahl-StickstoffsBoues, bio-déchets traités et sols - Détermination de l'azote KjeldahlSludge, treated biowaste and soil - Determination of Kjeldahl nitrogen13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16169:2012SIST EN 16169:2013en,fr,de01-februar-2013SIST EN 16169:2013SLOVENSKI

STANDARD
SIST EN 16169:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16169
August 2012 ICS 13.030.01; 13.080.10 English Version
Sludge, treated biowaste and soil - Determination of Kjeldahl nitrogen
Boues, bio-déchets traités et sols - Détermination de l'azote Kjeldahl

Schlamm, behandelter Bioabfall und Boden - Bestimmung des Kjeldahl-Stickstoffs This European Standard was approved by CEN on 24 May 2012.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,

B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16169:2012: ESIST EN 16169:2013

EN 16169:2012 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41 Scope ......................................................................................................................................................52 Normative references ............................................................................................................................53 Terms and definitions ...........................................................................................................................54 Principle ..................................................................................................................................................55 Interferences and sources of errors ....................................................................................................66 Reagents .................................................................................................................................................67 Apparatus ...............................................................................................................................................78 Sample storage and sample pretreatment ..........................................................................................79 Procedure ...............................................................................................................................................79.1 General ....................................................................................................................................................79.2 Digestion .................................................................................................................................................79.3 Titration ...................................................................................................................................................89.4 Performance check ................................................................................................................................89.5 Blank test ................................................................................................................................................810 Calculation ..............................................................................................................................................811 Expression of results ............................................................................................................................912 Precision .................................................................................................................................................913 Test report ..............................................................................................................................................9Annex A (informative)

Repeatability and reproducibility data ..................................................................... 10A.1 Materials used in the interlaboratory comparison study ............................................................... 10A.2 Interlaboratory comparison results .................................................................................................. 11Bibliography ..................................................................................................................................................... 12 SIST EN 16169:2013

EN 16169:2012 (E) 3 Foreword This document (EN 16169:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee - Horizontal standards in the fields of sludge, biowaste and soil”, 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 identical text or by endorsement, at the latest by February 2013, and conflicting national standards shall be withdrawn at the latest by February 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The preparation of this document by CEN is based on a mandate by the European Commission (Mandate M/330), which assigned the development of standards on sampling and analytical methods for hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

SIST EN 16169:2013

EN 16169:2012 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see also Annex A for the results of the validation). Table 1 — Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Fresh compost Compost Soil Sludge amended soil Agricultural soil

WARNING — Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT — It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff.

SIST EN 16169:2013

EN 16169:2012 (E) 5 1 Scope This European Standard specifies the determination of Kjeldahl nitrogen according to the Kjeldahl procedure in sludge, treated biowaste and soil. Nitrate and nitrite are not included.

Compounds with nitrogen bound in N-N, N-O linkages and some heterocycles (pyridines) are only partially determined. The limit of detection (LOD) is usually 0,03 % nitrogen, and the limit of quantification (LOQ) is 0,1 % nitrogen (using 0,25 mol/l sulfuric acid for titration). 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after determination of dry residue or water content EN 16179, Sludge, treated biowaste and soil —– Guidance for sample pretreatment EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) EN ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge and sediment samples (ISO 5667-15) ISO 18512, Soil quality — Guidance on long and short term storage of soil samples 3 Terms and definitions For the purpose of this document, the following terms and definitions apply. 3.1 Kjeldahl nitrogen nitrogen that is contributed by free ammonia, inorganic ammonia compounds and those types of organic nitrogen compounds that are converted to ammonium sulfate by the digestion process described in this standard (catalytic sulfuric acid digestion) [SOURCE: EN 13342:2000, 3.1] 4 Principle The dried and homogenized, moist or liquid material is digested in a suitable Kjeldahl tube with sulfuric acid, thus converting most nitrogen compounds present to ammonium sulfate. To raise the temperature, potassium sulfate is added and e.g. a mixture of titanium dioxide and copper sulfate is used as a catalyst. After adding sodium hydroxide to the digestion solution the produced ammonium is evaporated by distillation as ammonia. This is condensed in the cooling system and flows into a conical flask with boric acid solution (or diluted sulfuric acid). This solution is analyzed for ammonia by titration with sulfuric or hydrochloric acid. SIST EN 16169:2013

EN 16169:2012 (E) 6 5 Interferences and sources of errors The Kjeldahl method in principle does not capture all nitrogen compounds. The nitrogen that occurs in N-N and N-O linkages (e.g. azo-, nitro- and nitroso compounds, hydrazines, hydrazones, oximes, pyrazolones, isooxazoles, dia- and triazines) is not completely recorded. Furthermore the inorganic fraction (nitrate and nitrite) is not determined. Another source of error includes contamination of the apparatus. Therefore the apparatus shall be rinsed after each analytical series and blank determinations shall be carried out. The amount of sulfuric acid used in digestion process depends on the composition of the sample (see Table 2). A ratio of sample to acid of at least 1:10 (ratio weight to volume) shall be used for samples with high content of organic

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