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, biodéchets 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
Publication Date
21-Aug-2012
Current Stage
9093 - Decision to confirm - Review Enquiry
Start Date
11-Jul-2024
Completion Date
14-Apr-2025

Overview

EN 16169:2012 is a European Standard developed by the CEN Technical Committee CEN/TC 400, focusing on the determination of Kjeldahl nitrogen in sludge, treated biowaste, and soil samples. The standard outlines the Kjeldahl procedure, a well-established analytical method that quantifies nitrogen primarily in organic and ammonia forms. This standard excludes nitrate and nitrite nitrogen and partially measures nitrogen in compounds with N-N, N-O linkages and certain heterocyclic compounds.

The method specifies the procedures for sample digestion, ammonia distillation, and titration, with detection limits typically around 0.03% nitrogen (LOD) and quantification limits near 0.1% nitrogen (LOQ). EN 16169:2012 is applicable across a wide range of materials including municipal sludge, fresh compost, agricultural soil, and sludge-amended soil.


Key Topics

  • Scope: Kjeldahl nitrogen determination in environmental matrices-sludge, treated biowaste, and soil.
  • Exclusions: Does not include nitrate and nitrite nitrogen content.
  • Principle: Catalytic sulfuric acid digestion converts nitrogen-containing compounds to ammonium sulfate, followed by ammonia distillation and titrimetric quantification.
  • Reagents and Apparatus:
    • Use of sulfuric acid, catalyst mixture (potassium sulfate, copper sulfate, titanium dioxide), sodium hydroxide, and boric acid solution.
    • Kjeldahl digestion flasks, digestion stands, and distillation apparatus such as Parnas-Wagner type recommended.
  • Sample Storage and Pretreatment:
    • Soil samples stored as per ISO 18512.
    • Sludge samples stored according to EN ISO 5667-15.
    • Pretreatment following EN 16179 to ensure homogeneity.
  • Detection Limits:
    • Limit of detection (LOD): ~0.03% nitrogen.
    • Limit of quantification (LOQ): ~0.1% nitrogen.
  • Calculation and Reporting:
    • Nitrogen content calculated using volumetric titration data and sample dry mass.
    • Results expressed in mg/kg or % nitrogen relative to dry matter with two significant figures.
  • Interferences and Errors:
    • Partial determination for nitrogen in some organic compounds.
    • Contamination risks addressed by rigorous apparatus cleaning and blank testing.
  • Performance and Precision:
    • Validated through interlaboratory comparisons.
    • Quality control via substances with known nitrogen contents, e.g., ammonium sulfate.

Applications

EN 16169:2012 serves as a vital standard for laboratories and environmental agencies engaged in the chemical analysis of:

  • Waste Treatment Monitoring: Assessing nitrogen content in municipal sludge and treated biowaste ensures compliance with environmental regulations.
  • Soil Fertility and Quality Analysis: Provides accurate nitrogen measurements critical for evaluating soil nutrient status in agriculture and land management.
  • Composting Process Control: Helps monitor nitrogen transformation during composting to optimize biological treatment processes.
  • Environmental Impact Assessment: Supports ecological studies by quantifying nitrogen in soils and waste materials, aiding in pollution control.
  • Research and Development: Standardized nitrogen determination helps in the development of new waste management and soil amendment products.

This method is suited for both research and routine analysis, requiring properly trained staff to ensure accuracy and reproducibility.


Related Standards

  • EN 16179: Guidance for sample pretreatment of sludge, treated biowaste, and soil-complements EN 16169 by addressing preparatory steps.
  • EN 15934: Calculation of dry matter fraction for sludge, biowaste, and soil-important for expressing nitrogen content relative to dry weight.
  • ISO 18512: Soil quality-guidance on storage protocols-for maintaining sample integrity before analysis.
  • EN ISO 5667-15: Water quality-sampling guidance specific to sludge and sediment samples-ensures representative and reliable sample collection.
  • EN 25663 and EN ISO 11732: Alternative or complementary methods for nitrogen measurement, including automated spectrophotometric procedures.
  • EN 13342:2000: Definition of Kjeldahl nitrogen-provides terminology used in EN 16169.

Keywords: EN 16169:2012, Kjeldahl nitrogen determination, sludge analysis, treated biowaste, soil nitrogen testing, Kjeldahl procedure, nitrogen quantification, environmental standards, waste monitoring, soil fertility assessment, CEN standards.

Standard
EN 16169:2013
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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
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

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

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.
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
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Frequently Asked Questions

EN 16169:2012 is a standard published by the European Committee for Standardization (CEN). Its full title is "Sludge, treated biowaste and soil - Determination of Kjeldahl nitrogen". This standard covers: 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).

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).

EN 16169:2012 is classified under the following ICS (International Classification for Standards) categories: 13.030.01 - Wastes in general; 13.080.10 - Chemical characteristics of soils. The ICS classification helps identify the subject area and facilitates finding related standards.

EN 16169:2012 is associated with the following European legislation: EU Directives/Regulations: 86/278/EEC; Standardization Mandates: M/330. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

You can purchase EN 16169:2012 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of CEN standards.

EN 16169:2012は、スラッジ、処理されたバイオ廃棄物および土壌におけるケルダール窒素の測定方法を規定した欧州規格であり、その適用範囲は非常に重要です。この規格は、環境管理や農業分野において、窒素の評価が欠かせないという現実を踏まえており、特にケルダール法による測定方法の標準化に寄与しています。また、窒素化合物の一部(N-N、N-O結合およびピリジンのようなヘテロ環式化合物)については一部しか測定できないことが明記されており、標準の限界を理解する手助けとなります。 この文書は、検出限界(LOD)が通常0.03%窒素、定量限界(LOQ)が0.1%窒素と詳細に規定されているため、実際の分析作業を行う上での指針としても非常に有用です。特に土壌やバイオ廃棄物の管理においては、正確な窒素測定が作物の成長に直接影響するため、その信頼性は業界の信頼を集めます。また、処理技術の進歩が求められる現代において、EN 16169:2012は持続可能な農業実践及び環境保護の観点からも大変関連性が高いです。 この規格に従うことで、関係者は一貫した結果を得ることができ、成果物の質を向上させることが期待できます。特に、環境保護の観点から、正確な窒素の把握は重要であり、もって生態系への影響を抑えるための一助となります。従って、EN 16169:2012はその適用範囲や実務への影響において、非常に価値のある基準であると言えます。

SIST EN 16169:2013은 슬러지, 처리된 생물 폐기물 및 토양에서의 켈달 질소(Kjeldahl nitrogen) 측정에 대해 상세히 규정하고 있는 유럽 표준으로, 해당 표준의 범위는 이러한 물질에서의 켈달 절차에 따른 질소 함량을 결정하는 것을 명확히 하고 있습니다. 이 표준은 식물 및 토양 과학 분야에서 중요한 역할을 하며, 해당 분야에서 생물학적 분해 과정을 이해하는 데 필수적인 도구입니다. SIST EN 16169:2013의 강점 중 하나는 측정의 신뢰성과 효율성을 제고하는 데 있습니다. 이 표준은 보통 0.03%의 질소 한계 검출 한계(LOD)와 0.1%의 질소 정량화 한계(LOQ)를 제공하여, 연구자들과 실무자들이 슬러지와 생물 폐기물에서 질소 함량을 정확하게 평가할 수 있도록 돕습니다. 특히, 이는 환경 모니터링 및 지속 가능한 관리 측면에서 매우 중요한 요소입니다. 또한, 해당 표준은 질소가 N-N, N-O 결합 형태로 결합되어 있는 화합물과 일부 이종 고리 화합물(예: 피리딘)의 제한적인 측정을 포함하고 있어, 특정 조건에서 화합물의 구성 성분에 대한 통찰력을 제공합니다. 이러한 부분은 특정 연구와 분석에 필요한 정보를 제공하며, 다양한 생태계에서 질소 순환의 복잡성을 이해하는 데 기여합니다. SIST EN 16169:2013은 환경 보호와 자원 관리를 위한 필수적인 기준으로 자리 잡고 있으며, 특히 슬러지 및 생물 폐기물 처리에 있어서 중요한 참고 자료로 활용됩니다. 이 표준이 제공하는 측정 방식과 기술적 요구사항은 보다 나은 환경 관리 및 연구 기반을 마련하는 데 큰 도움이 될 것입니다.

La norme EN 16169:2012, intitulée "Boues, bioproduits traités et sols - Détermination de l'azote Kjeldahl", constitue un cadre essentiel pour l'analyse de la composition azotée des boues et des déchets organiques traités. Son champ d'application précis permet de se concentrer sur la détermination de l'azote Kjeldahl grâce à une méthode bien établie, ce qui en fait un outil précieux pour les laboratoires et les professionnels du secteur environnemental. Parmi les forces de cette norme, on note la clarté des procédures établies qui garantissent une répétabilité des résultats dans l'évaluation de la qualité des échantillons. La méthode Kjeldahl est largement reconnue et, en intégrant des limites de détection (LOD) de 0,03 % d'azote et des limites de quantification (LOQ) de 0,1 % d'azote, la norme assure une sensibilisation accrue dans les analyses de très faibles concentrations d'azote, un aspect crucial pour les études environnementales et agricoles. Cependant, il est important de mentionner que la norme ne traite pas des nitrates et des nitrites, ce qui pourrait limiter l'analyse globale des composés azotés dans certains contextes. De plus, les composés azotés liés à des liaisons N-N, N-O et certains hétérocycles sont seulement partiellement déterminés, ce qui peut poser des défis dans des applications spécifiques où une analyse complète de tous les types de composés azotés est nécessaire. En somme, la norme SIST EN 16169:2013 demeure un document de référence pertinent dans le domaine de l'analyse des boues, bioproduits traités et sols, offrant des méthodologies solides pour la quantification de l'azote Kjeldahl, tout en mettant en lumière des domaines d'amélioration pour des analyses futures.

The EN 16169:2012 standard is a comprehensive guideline that addresses the determination of Kjeldahl nitrogen in various matrices including sludge, treated biowaste, and soil. This European Standard is instrumental for laboratories engaged in environmental testing and assessment of nitrogen content, offering a standardized procedure that fosters consistency and accuracy in analytical practices. One of the key strengths of this standard is its clear delineation of its scope, emphasizing the focus on Kjeldahl nitrogen determination while specifically excluding nitrate and nitrite measurements. This specificity aids professionals in understanding the limitations and applicability of the method, ensuring that users are well-informed about what is and isn't covered under this standard. Additionally, the standard acknowledges that certain nitrogen compounds, particularly those bound in N-N, N-O linkages, and some heterocycles such as pyridines, are only partially determined. This transparency helps laboratories plan their analyses effectively, allowing for the necessary adjustments when interpreting results. Furthermore, the standard sets forth rigorous detection and quantification thresholds, with a limit of detection (LOD) typically at 0.03% nitrogen and a limit of quantification (LOQ) at 0.1% nitrogen using a 0.25 mol/l sulfuric acid for titration. These stringent parameters underscore the reliability of the Kjeldahl procedure, which is crucial for environmental monitoring and compliance, as the accurate measurement of nitrogen levels in substrates can have significant implications for soil health, waste management practices, and regulatory adherence. The relevance of EN 16169:2012 extends beyond mere compliance; it serves as a foundational tool for researchers and professionals aiming to understand the nitrogen cycle within ecological systems. By standardizing Kjeldahl nitrogen determination, the document enhances the comparability of data across various studies and regulatory frameworks, facilitating a more integrated approach to environmental management. In summary, EN 16169:2012 stands out as a vital standard in the field of environmental analysis. Its clear scope, stringent measurement criteria, and focus on Kjeldahl nitrogen make it an essential reference for laboratories and professionals committed to delivering reliable, high-quality results in the assessment of sludge, treated biowaste, and soil.

Die Norm EN 16169:2012 ist ein wichtiger Standard, der sich mit der Bestimmung von Kjeldahl-Stickstoff in Schlamm, behandeltem Biokraftstoff und Boden beschäftigt. Dieses Dokument legt die Methodik zur Durchführung des Kjeldahl-Verfahrens fest, welches für viele Anwendungen in der Umwelt- und Abfallwirtschaft von entscheidender Bedeutung ist. Der Umfang dieser Norm ist klar umrissen und bietet eine präzise Anleitung zur Bestimmung des Kjeldahl-Stickstoffs in verschiedenen Proben, was eine wesentliche Grundlage für die Analyse der Nährstoffverfügbarkeit in Böden und Abfällen darstellt. Die Tatsache, dass Nitrate und Nitrite nicht in die Analyse einbezogen werden, ist ebenfalls hervorzuheben, da dies die Konzentration auf die spezifischen Verbindungen lenkt, die durch das Kjeldahl-Verfahren gemessen werden können. Eine der Stärken dieser Norm ist die detaillierte Vorgehensweise, die es ermöglicht, zuverlässige und reproduzierbare Ergebnisse zu erzielen. Die Grenzwerte für die Nachweisgrenze (LOD) von 0,03 % Stickstoff und die Quantifizierungsgrenze (LOQ) von 0,1 % Stickstoff sind gut definiert und gewährleisten die Genauigkeit der Testergebnisse. Die Verwendung von 0,25 mol/l Schwefelsäure zur Titration verstärkt die Präzision des Verfahrens und macht die Norm besonders relevant für Laboranalysen. Die Relevanz der Norm EN 16169:2012 erstreckt sich über den rein analytischen Bereich hinaus und hat weitreichende Auswirkungen auf die Umweltüberwachung sowie das Management von Abfall und Biowaste. Durch die Bereitstellung eines klaren und konsistenten Rahmens unterstützt diese Norm Fachleute in verschiedenen Branchen, sichere und verantwortungsvolle Praktiken zu implementieren. Die Einhaltung dieses Standards ist für Unternehmen, die in der Abfall- und Umweltbranche tätig sind, unerlässlich, um die Qualität ihrer Analysen und die Übergabe von Beweisen zur Nachhaltigkeit sicherzustellen.