Sludge, treated biowaste and soil - Extraction for the determination of extractable ammonia, nitrate and nitrite

This Technical Specification specifies a procedure for the determination of ammonium nitrogen and nitrate nitrogen in sludge, treated biowaste and soil after extraction with a 1 mol/l potassium chloride solution. The extraction method is suitable for fresh samples.
The determination of nitrogen fractions can be done manually or by automated methods.

Schlamm, behandelter Bioabfall und Boden - Bestimmung von extrahierbarem Ammoniumstickstoff, Nitrat- und Nitritstickstoff

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung von Ammonium Stickstoff und Nitrat-Stickstoff in Schlamm, behandeltem Bioabfall und Boden nach der Extraktion mit einer 1 mol/l Kaliumchlorid-lösung fest. Das Extraktionsverfahren ist für frische Proben geeignet.
Die Bestimmung von Stickstoffanteilen kann manuell oder mithilfe automatisierter Verfahren vorgenommen werden.

Boues, biodéchets traités et sols - Extraction pour la détermination de l'azote nitrique et ammoniacal extractible

La présente Spécification technique définit un mode opératoire pour le dosage de l'azote ammoniacal et de l'azote nitrique dans les boues, les biodéchets traités et les sols après extraction avec une solution de chlorure de potassium à 1 mol/l. La méthode d'extraction convient pour les échantillons frais.
Le dosage des fractions azotées peut être effectué manuellement ou par des méthodes automatisées.

Blato, obdelani biološki odpadki in tla - Določevanje amonija, nitrata in nitrita, sposobnih ekstrakcije

Ta tehnična specifikacija opredeljuje postopek za določevanje amonijevega dušika in nitritovega dušika v blatu, obdelanih bioloških odpadkih in tleh po ekstrakciji z 1 mol/l raztopino kalijevega klorida. Metoda ekstrakcije je primerna za sveže vzorce. Določanje deležev dušika se lahko izvede ročno ali s samodejnimi metodami.

General Information

Status
Published
Publication Date
21-Feb-2012
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
30-Jun-2021

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SLOVENSKI STANDARD
SIST-TS CEN/TS 16177:2012
01-junij-2012

%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHDPRQLMDQLWUDWDLQQLWULWD

VSRVREQLKHNVWUDNFLMH

Sludge, treated biowaste and soil - Extraction for the determination of extractable

ammonia, nitrate and nitrite
Schlamm, behandelter Bioabfall und Boden - Bestimmung von extrahierbarem
Ammoniumstickstoff, Nitrat- und Nitritstickstoff

Boues, bio-déchets traités et sols - Extraction pour la détermination de l'azote nitrique et

ammoniacal extractible
Ta slovenski standard je istoveten z: CEN/TS 16177:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST-TS CEN/TS 16177:2012 en,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 16177:2012
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SIST-TS CEN/TS 16177:2012
TECHNICAL SPECIFICATION
CEN/TS 16177
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2012
ICS 13.030.01
English Version
Sludge, treated biowaste and soil - Extraction for the
determination of extractable ammonia, nitrate and nitrite

Boues, biodéchets traités et sols - Extraction pour la Schlamm, behandelter Bioabfall und Boden - Bestimmung

détermination de l'azote nitrique et ammoniacal extractible von extrahierbarem Ammoniumstickstoff, Nitrat- und

Nitritstickstoff

This Technical Specification (CEN/TS) was approved by CEN on 24 April 2011 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their

comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available

promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)

until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, 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 Ref. No. CEN/TS 16177:2012: E

worldwide for CEN national Members.
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SIST-TS CEN/TS 16177:2012
CEN/TS 16177:2012 (E)
Contents Page

Foreword ..............................................................................................................................................................3

Introduction .........................................................................................................................................................4

1 Scope ......................................................................................................................................................5

2 Normative references ............................................................................................................................5

3 Terms and definitions ...........................................................................................................................5

4 Principle ..................................................................................................................................................5

5 Interferences and sources of errors ....................................................................................................5

6 Reagents .................................................................................................................................................6

7 Apparatus ...............................................................................................................................................6

8 Procedure ...............................................................................................................................................6

8.1 Preparation .............................................................................................................................................6

8.2 Extraction ...............................................................................................................................................6

8.3 Filtration ..................................................................................................................................................7

8.4 Determination .........................................................................................................................................7

8.5 Calibration ..............................................................................................................................................7

8.6 Blank determination ..............................................................................................................................7

9 Calculation and expression of results .................................................................................................7

9.1 Method of calculation ............................................................................................................................7

9.2 Expression of results ............................................................................................................................7

10 Precision .................................................................................................................................................7

11 Test report ..............................................................................................................................................8

Annex A (informative) Repeatability and reproducibility data ........................................................................9

A.1 Materials used in the interlaboratory comparison study ..................................................................9

A.2 Interlaboratory comparison results .................................................................................................. 10

Annex B (informative) Performance data ....................................................................................................... 11

Bibliography ..................................................................................................................................................... 13

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SIST-TS CEN/TS 16177:2012
CEN/TS 16177:2012 (E)
Foreword

This document (CEN/TS 16177:2012) 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.

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.

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 announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,

Czech Republic, Denmark, Estonia, Finland, 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.
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SIST-TS CEN/TS 16177:2012
CEN/TS 16177:2012 (E)
Introduction

This Technical Specification 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 Technical Specification 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 Technical Specification should be familiar with usual laboratory

practice. This Technical Specification 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 Technical

Specification be carried out by suitably trained staff.
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SIST-TS CEN/TS 16177:2012
CEN/TS 16177:2012 (E)
1 Scope

This Technical Specification specifies a procedure for the determination of ammonium nitrogen and nitrate

nitrogen in sludge, treated biowaste and soil after extraction with a 1 mol/l potassium chloride solution. The

extraction method is suitable for fresh samples.

The determination of nitrogen fractions can be done manually or by automated methods.

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 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 11732, Water quality — Determination of ammonium nitrogen — Method by flow analysis (CFA and

FIA) and spectrometric detection (ISO 11732)

ISO 7150-1, Water quality — Determination of ammonium — Part 1: Manual spectrometric method

ISO 14256-2, Soil quality — Determination of nitrate, nitrite and ammonium in field-moist soils by extraction

with potassium chloride solution — Part 2: Automated method with segmented flow analysis

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
nitrogen fractions

mass of ammonium nitrogen and nitrate nitrogen (mineral nitrogen) that is released after a single or repeated

extraction of the sample using 1 mol/l potassium chloride solution
4 Principle

An aliquot of the homogenised fresh material is shaken for 1 h with 1 mol/l potassium chloride solution at room

temperature. The ratio of extractant to material varies according to the material tested. The extraction solution

is centrifuged or filtered and an aliquot of the filtrate is analysed by flow injection analysis (FIA) or continuous

flow analysis (CFA) or by manual methods as distillation and titration or spectrophotometric method.

5 Interferences and sources of errors

The samples can change composition due to biological and/or chemical activity. The fresh or the deep frozen

homogenised test sample is directly transferred to the extraction bottle, which is filled with the potassium

chloride solution, if a change in the content of the nitrogen fractions can be expected. Drying of the material,

even rapid microwave drying will result in a change of the nitrogen content especially of ammonium. Take

care to use purified glassware and equipment and filter papers free of contaminations with nitrate and

ammonium. Cleaning of glassware with water shall be performed after each use, especially to avoid cross

contaminations from samples with high contents of nitrogen fractions, like sludge or biowaste. Use separate

equipment for the analysis of soil samples, as contents of nitrogen fractions can be near the detection limit. A

blank test shall be carried out to assure purity of reagents and equipment.
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CEN/TS 16177:2012 (E)
6 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
6.1 Water, grade 2 according to EN ISO 3696.
6.2 Potassium chloride, c(KCl) = 1 mol/l.
Dissolve 373 g of KCl, dried at 105 °C, in approximately 3 l wate
...

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