SIST EN 16169:2013
(Main)Sludge, treated biowaste and soil - Determination of Kjeldahl nitrogen
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
- KAT - Soil quality
- Current Stage
- 6060 - National Implementation/Publication (Adopted Project)
- Start Date
- 04-Jan-2013
- Due Date
- 11-Mar-2013
- Completion Date
- 21-Jan-2013
Overview
SIST EN 16169:2013 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). SIST EN 16169:2013 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
SIST EN 16169:2013 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: SIST EN 16169:2013, Kjeldahl nitrogen determination, sludge analysis, treated biowaste, soil nitrogen testing, Kjeldahl procedure, nitrogen quantification, environmental standards, waste monitoring, soil fertility assessment, CEN standards.
Frequently Asked Questions
SIST EN 16169:2013 is a standard published by the Slovenian Institute for Standardization (SIST). 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).
SIST EN 16169:2013 is classified under the following ICS (International Classification for Standards) categories: 13.030.20 - Liquid wastes. Sludge; 13.080.10 - Chemical characteristics of soils. The ICS classification helps identify the subject area and facilitates finding related standards.
SIST EN 16169:2013 is associated with the following European legislation: EU Directives/Regulations: 86/278/EEC, TP136; 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.
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Standards Content (Sample)
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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Die Norm SIST EN 16169:2013 bietet eine präzise und umfassende Vorgehensweise zur Bestimmung des Kjeldahl-Stickstoffs in Schlamm, behandeltem Biowaste und Boden. Der Fokus auf das Kjeldahl-Verfahren stellt sicher, dass eine zuverlässige Analyse in relevanten Proben durchgeführt wird. Der Anwendungsbereich dieser Norm ist klar definiert, was in der Praxis von großem Nutzen ist. Es wird spezifisch auf die Analysemethoden für Schlamm und behandelten Biowaste eingegangen, was die Relevanz für Umweltanalytik und Abfallmanagement erhöht. Zudem wird erklärt, dass Nitrat und Nitrit nicht erfasst werden, was für Anwender wichtig ist, um eine maßgeschneiderte Analyse durchzuführen und Missverständnisse zu vermeiden. Ein bedeutender Aspekt der Norm ist die Genauigkeit der Detektionsgrenzen. Mit einer Nachweisgrenze (LOD) von 0,03 % Stickstoff und einer Bestimmungsgrenze (LOQ) von 0,1 % Stickstoff bei der Verwendung von 0,25 mol/l Schwefelsäure für die Titration, bietet die Norm eine solide Grundlage für qualitativ hochwertige Datenerhebung. Diese Werte gewährleisten, dass selbst niedrige Konzentrationen von Stickstoff nachgewiesen werden können, was für viele Anwendungen in der Umweltwissenschaft von entscheidender Bedeutung ist. Die Norm berücksichtigt auch die Einschränkungen bei der Bestimmung von Stickstoffverbindungen, die in N-N- oder N-O-Bindungen und einigen Heterocyclen (wie Pyridinen) vorkommen. Dies zeigt das Engagement, eine realistische und anwendbare Methode für die Bestimmung von Kjeldahl-Stickstoff bereitzustellen, während gleichzeitig klargestellt wird, welche Verbindungen nur teilweise erfasst werden können. Insgesamt stellt die SIST EN 16169:2013 eine wertvolle Referenz in der analytischen Chemie dar, insbesondere im Hinblick auf die Bestimmung des Kjeldahl-Stickstoffs in relevanten Umweltdaten. Die Stärke dieser Norm liegt in ihrer klaren Struktur und den detaillierten Vorgaben, die Fachleuten helfen, präzise und verlässliche analytische Ergebnisse zu erzielen.
SIST EN 16169:2013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Kjeldahl窒素の測定を規定した欧州標準です。この標準の主な範囲は、Kjeldahl手法に基づいて窒素を測定することに重点を置いており、スラッジや処理されたバイオ廃棄物、土壌の分析に非常に重要です。また、この標準は硝酸塩や亜硝酸塩を含まず、N-N、N-O結合に結合した窒素および一部のヘテロ環式化合物（ピリジン）を部分的にしか測定しないことを明確にしています。 この標準の強みは、高い精度と信頼性を持つ窒素測定法を提供している点にあります。限界値も明示されており、検出限界（LOD）は通常0.03 %窒素、定量限界（LOQ）は0.1 %窒素であり、0.25 mol/l硫酸を使用した滴定によって達成されます。これにより、研究者や技術者は必要な感度を持つ測定を行うことができ、景観保全や環境監視において非常に効果的です。 この標準は、環境科学、土壌科学、農業などの分野において、窒素の状態を理解し、管理する上で不可欠です。従って、SIST EN 16169:2013は、持続可能な開発や環境保護の観点からも非常に関連性の高い文書であり、関係者にとって価値のあるリソースとなるでしょう。
La norme SIST EN 16169:2013 est une référence essentielle pour la détermination de l'azote Kjeldahl dans les boues, les déchets organiques traités et le sol. Son domaine d'application est clairement défini, se concentrant sur la méthode Kjeldahl, mais excluant les nitrates et nitrites, ce qui la rend particulièrement pertinente dans des contextes où la mesure précise de ces éléments est primordiale. Parmi ses points forts, la norme établit des limites de détection et de quantification claires, respectivement de 0,03 % et 0,1 % d'azote. Cela assure aux laboratoires la fiabilité et l'exactitude nécessaires lors de l'analyse des échantillons de boues et de déchets organiques. En outre, l'utilisation d'acide sulfurique à 0,25 mol/l pour la titration renforce la robustesse de la méthode décrite. La norme est également pertinente dans le domaine de l'analyse environnementale, permettant une évaluation précise de la qualité des sols et des déchets, éléments cruciaux dans la gestion durable des ressources. La partialité de la détermination de certains composés azotés, tels que ceux liés par des liaisons N-N et N-O, ainsi que certains hétérocycles comme les pyridines, souligne la nécessité d'interpréter les résultats dans un contexte plus large. En somme, la SIST EN 16169:2013 se positionne comme un standard indispensable pour la détermination de l'azote Kjeldahl, garantissant des méthodes d'analyse solides et adaptées aux exigences contemporaines du secteur environnemental.
SIST EN 16169:2013 표준은 슬러지, 처리된 바이오 폐기물 및 토양에서의 켈달 질소(Kjeldahl nitrogen) 측정을 위한 유럽 표준으로, 이 표준은 질소가 포함된 화합물의 정밀한 분석을 목적으로 하고 있습니다. 이 문서는 켈달 방법에 따른 질소 측정 절차를 명확하게 규정하고 있어, 관련 분야에서 매우 중요한 역할을 합니다. 이 표준의 강점 중 하나는 질소의 존재량을 정확하고 신뢰성 있게 측정할 수 있다는 점입니다. 일반적으로 감지 한계(LOD)는 0.03% 질소, 정량 한계(LOQ)는 0.1% 질소로 설정되어 있어, 저농도의 질소도 효과적으로 검출할 수 있습니다. 이러한 정밀도는 환경 모니터링, 농업 및 폐기물 관리 분야에서 필수적이며, 특히 토양의 질소 관리와 에코시스템 건강을 평가하는 데 중요한 역할을 합니다. SIST EN 16169:2013 표준은 또한 슬러지와 처리된 바이오 폐기물, 그리고 토양 내 질소를 측정하는 효과적인 방법을 제시하여, 다양한 산업 및 연구에서 활용될 수 있는 기본적인 지침을 제공합니다. 이러한 표준은 질소의 비율을 정확히 평가할 수 있는 기초를 제공함으로써, 지속 가능한 발전 및 환경 보호 노력에 기여하고 있습니다. 그러나, 이 표준은 질산염(nitrate) 및 아질산염(nitrite)은 포함하지 않으며, 일부 질소가 결합된 화합물(N-N, N-O 연결 및 일부 헤테로사이클) 또한 부분적으로만 분석됩니다. 이로 인해 특정 환경적 요구 사항에 부합하지 않을 수 있으므로, 사용자들은 이를 인지하고 활용해야 합니다. 결론적으로, SIST EN 16169:2013 표준은 슬러지 및 바이오 폐기물 관리 분야에서 요구되는 질소 분석의 핵심적인 기준을 제공하여, 연구자와 전문인들이 실질적인 결과를 도출하는 데 기여하는 유용한 문서라고 할 수 있습니다.
The SIST EN 16169:2013 standard is a pivotal document that delineates the methodology for the determination of Kjeldahl nitrogen in sludge, treated biowaste, and soil. Its scope is explicitly tailored to the Kjeldahl procedure, effectively addressing a significant aspect of nitrogen analysis in these materials. One of the strengths of this standard is its clarity in outlining the limitations of the methodology, including the exclusion of nitrate and nitrite, which are commonly found nitrogen species in environmental matrices. Additionally, it provides insight into the partial determination of certain nitrogen compounds, such as those bound in N-N and N-O linkages and specific heterocycles like pyridines. This level of detail is essential for practitioners in the field, ensuring they understand the method's applicability and constraints. The standard also specifies critical parameters like the limit of detection (LOD) and the limit of quantification (LOQ) at 0.03% nitrogen and 0.1% nitrogen, respectively, using a 0.25 mol/l sulfuric acid for titration. These quantitative benchmarks provide indispensable guidance for laboratories, facilitating accurate and reliable nitrogen measurements in the specified matrices. Overall, SIST EN 16169:2013 stands out for its comprehensive approach to the determination of Kjeldahl nitrogen, making it a highly relevant standard for environmental scientists, waste management professionals, and soil scientists engaged in assessing nutrient content and environmental quality. The standard's focus on precision and clarity enhances its utility in practical applications, fostering consistency and reliability in nitrogen determination across various environmental contexts.
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