CEN/TS 16177:2012

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

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.

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

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.
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.
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.
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 water (6.1) and dilute to 5 l with water (6.1).
7 Apparatus
Usual laboratory apparatus, and in particular the following:
7.1 Analytical balance with an accuracy of at least 0,01 g.
7.2 Wide necked glass or plastic bottles with secure stopper or caps, nominal volume 250 ml or
500 ml or other.
The material shall not adsorb ammonium, nitrate or nitrite and shall not be contaminated with these
compounds.
–1 –1
7.3 Shaking apparatus, end-over-end shaker, frequency 30 min to 40 min or other appropriate shakers.
7.4 Filter paper, free of nitrogen fractions, pore size 8 µm to 12 µm.
8 Procedure
8.1 Preparation
Pretreat the samples according to EN 16179, if not otherwise specified.
When the content of mineral nitrogen is determined in deep-frozen samples, the temperature and the duration
of the thawing process shall be controlled. The samples can be thawed at room temperature, if they are
homogenised and extracted within 4 h after beginning of thawing. Thawing at 4 °C is also possible, but the
thawing period should not exceed 48 h. The fresh test sample can be homogenised by manual methods which
shall be performed in a way that avoids contamination of the test sample with nitrogen fractions.
NOTE The use of gloves is recommended when homogenising test samples.
8.2 Extraction
Transfer a known amount of the homogenised test sample (equal to 1,0 g to 10,0 g dry mass) into an
extraction bottle (7.2), add potassium chloride solution (6.2) in a mass (dry mass of the sample, m) to volume
(of the extracting solution, V) ratio of (m/V):
 1 to 5 (m/V) for field moist fresh soil (< 10 mm); or
 1 to 10 (m/V) for dry soil samples (< 2 mm); and
 1 to 20 up to 1 to 80 (m/V) for treated biowaste, sludge or sludge amended soils.
Close the bottle cap and place the extraction bottle in the shaking apparatus (7.3). Shake it for 1 h at room
temperature. A minimum of one repetiti
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