CEN/TS 17174:2018
(Main)Animal feeding stuffs: Methods of sampling and analysis - Performance criteria for single laboratory validated and ring-trial validated methods of analysis for the determination of heavy metals
Animal feeding stuffs: Methods of sampling and analysis - Performance criteria for single laboratory validated and ring-trial validated methods of analysis for the determination of heavy metals
This document specifies performance criteria for the selection of single-laboratory validated or collaborative-trial validated methods of analysis of elements and their chemical species in feed. The terms and definition of the relevant parameters for method validation are included. The performance requirements and characteristics are provided. This document may serve as a guide:
- to assess the quality of new European Standard methods under validation;
- to review the quality of previous collaborative trials;
- to confirm the extension of the scope of an already published European Standard applied to other analyte concentrations or matrices; or
- to evaluate the fitness-for-purpose of single-validated methods.
The performance criteria can apply to methods dedicated to the determination of heavy metals, trace elements, major elements and minerals.
Futtermittel - Probenahme- und Untersuchungsverfahren - Leistungskriterien für laborintern validierte und Ringversuch validierte Analysemethoden zur Bestimmung von Schwermetallen
Dieses Dokument legt Leistungskriterien für die Auswahl von in Einzellaboratorien validierten oder in Laborvergleichsuntersuchungen validierten Analyseverfahren für Elemente und ihren Verbindungen in Futtermitteln fest. Enthalten sind die Begriffe der relevanten Parameter für die Verfahrensvalidierung. Die Leistungsanforderungen und merkmale werden zur Verfügung gestellt. Dieses Dokument darf als Orientierung dienen für:
- die Beurteilung der Qualität neuer Europäischer Normverfahren während ihrer Validierung;
- die Überprüfung der Qualität vorangegangener Laborvergleichsuntersuchungen;
- die Bestätigung der Erweiterung des Anwendungsbereichs einer bereits veröffentlichten Europäischen Norm, die für andere Analytkonzentrationen oder Matrices angewendet wurde; oder
- die Evaluierung der Gebrauchseignung einfach validierter Verfahren.
Die Leistungskriterien können bei Verfahren zur Bestimmung von Schwermetallen, Spurenelementen, Hauptelementen und Mineralien verwendet werden.
Aliments des animaux : Méthodes d’échantillonnage et d’analyse - Critères de performance pour les méthodes d’analyse validées par un ou plusieurs laboratoires pour le dosage des métaux lourds
Le présent document spécifie les critères de performance pour la sélection de méthodes validées par un ou plusieurs laboratoires pour l’analyse des éléments minéraux et de leurs espèces chimiques dans les aliments composés pour animaux. Les termes et définitions de paramètres pertinents pour la validation des méthodes sont inclus. Les exigences de performance et les caractéristiques sont fournies. Le présent document peut servir de guide :
- pour évaluer la qualité des nouvelles méthodes de Norme européenne en cours de validation ;
- pour examiner la qualité de précédents essais interlaboratoires ;
- pour confirmer l’extension du domaine d’application d’une Norme européenne déjà publiée appliquée à d’autres concentrations ou matrices d’analytes ; ou
- pour évaluer l’adaptation à l’objectif de méthodes validées par un seul laboratoire.
Les critères de performance peuvent s’appliquer aux méthodes dédiées au dosage des métaux lourds, des éléments trace, des éléments majeurs et des minéraux.
Krma: metode vzorčenja in analize - Izvedbena merila v posameznem laboratoriju in v primerjalnem preskusu validirane metode analiz za določanje težkih kovin
Ta dokument določa izvedbena merila za izbiro v posameznem laboratoriju ali primerjalnem preskusu validiranih metod analiz elementov in njihovih kemičnih vrst v krmi. Vključeni so izrazi in opredelitve ustreznih parametrov v zvezi za validacijo metode. Podane so tudi zahteve za izvedbo in lastnosti. Ta dokument se lahko uporablja kot vodnik za:
– ocenjevanje kakovosti metod novih evropskih standardov v postopku validacije;
– pregled kakovosti prejšnjih primerjalnih preskusov;
– potrditev razširitve področja uporabe že objavljenega evropskega standarda, ki se uporablja za druge koncentracije ali matrice analita; ali
– vrednotenje primernosti za namen v posameznem laboratoriju validiranih metod.
Izvedbena merila je mogoče uporabljati za metode, ki so namenjene določanju težkih kovin, elementov v sledovih ter glavnih elementov in mineralov.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-oktober-2018
.UPD PHWRGHY]RUþHQMDLQDQDOL]H,]YHGEHQDPHULODYSRVDPH]QHPODERUDWRULMX
LQYSULPHUMDOQHPSUHVNXVXYDOLGLUDQHPHWRGHDQDOL]]DGRORþDQMHWHåNLKNRYLQ
Animal feeding stuffs: Methods of sampling and analysis - Performance criteria for single
laboratory validated and ring-trial validated methods of analysis for the determination of
heavy metals
Futtermittel - Probenahme- und Untersuchungsverfahren - Leistungskriterien für
laborintern validierte und Ringversuch validierte Analysemethoden zur Bestimmung von
Schwermetallen
Aliments des animaux : Méthodes d'échantillonnage et d'analyse - Critères de
performance pour les méthodes d'analyse validées par un ou plusieurs laboratoires pour
le dosage des métaux lourds
Ta slovenski standard je istoveten z: CEN/TS 17174:2018
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN/TS 17174
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
August 2018
TECHNISCHE SPEZIFIKATION
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Performance criteria for single laboratory validated and
ring-trial validated methods of analysis for the
determination of heavy metals
Aliments des animaux : Méthodes d'échantillonnage et Futtermittel - Probenahme- und
d'analyse - Critères de performance pour les méthodes Untersuchungsverfahren - Leistungskriterien für
d'analyse validées par un ou plusieurs laboratoires laborintern validierte und Ringversuch validierte
pour le dosage des métaux lourds Analysemethoden zur Bestimmung von
Schwermetallen
This Technical Specification (CEN/TS) was approved by CEN on 8 February 2018 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17174:2018 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Criteria for analytical methods for heavy metals . 13
4.1 Overall concepts . 13
4.2 Horwitz/Thompson equation . 13
4.3 Horwitz ratio . 14
4.4 Precision . 14
4.5 Trueness . 15
4.6 Minimum applicability range . 15
4.7 Limit of detection (LOD) and limit of quantification (LOQ) . 16
Annex A (normative) Review of the repeatability and reproducibility relative standard
deviations reported in the EN 15510 standard and EN 15621 technical specifications . 17
Annex B (informative) R and RSD versus mass fractions . 21
rec
Annex C (informative) Assessment of method compliance. 23
Bibliography . 25
European foreword
This document (CEN/TS 17174:2018) has been prepared by Technical Committee CEN/TC 327 “Animal
feeding stuffs: Methods of sampling and analysis”, the secretariat of which is held by NEN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN 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.
According to the CEN/CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to announce this Technical Specification: 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom
Introduction
The working group, CEN/TC 327 “Animal feeding stuffs - Methods of sampling and analysis” WG 4
“Elements and their chemical species” selects and elaborates methods of analysis of elements and their
chemical species in feedstuffs.
There are many methods of analysis for the determination of elements in feedstuffs, which have been
validated and published. It is often required to make a choice between several established methods
applicable to the same measurand (analyte/matrix combination).
The Working Group was mandated by the European Commission [1] to establish specific criteria to
guide the analyst in the selection between several methods of analysis. As a general rule, analysts
should give preference to methods of analysis which comply with the provisions given in Clauses 1 and
2 of Annex III to the Regulation (EU) 2017/625 [2], in the Directive 2002/32/EC [3], with the
Commission Regulation (EC) No 152/2009 [4], or with the General Principles for Methods of Analysis of
the Codex Alimentarius Commission (CAC), as defined in the CAC Procedural Manual [5] and further
developed in the “criteria approach” to the methods of analysis developed by the Codex Committee of
Methods of Analysis and Sampling (CCMAS) [6].
The performance criteria laid down in this document are based on published guidance documents (such
as the AOAC guidelines [7]; the IUPAC Harmonized Protocol [8] and the SANCO document [9]) or data
collected from official reports on European collaborative studies (e.g. EN 15510 [10] or EN 15621 [11]).
When such performance characteristics are not available, the criteria were established based on the
experience and opinions of the CEN/TC 327/WG 4.
The criteria included in this document have also been used as guidance in the Working Group for the
selection of specific methods of analysis of trace elements to be further standardized, for the evaluation
of on-going collaborative trials and for the review of previously published standards of analytical
methods.
NOTE All the criteria provided in this document refer to concentrations (mass fractions) greater than or
equal to 0,1 mg/kg, related to the lowest maximum level (ML) set for mercury in feed.
1 Scope
This document specifies performance criteria for the selection of single-laboratory validated or
collaborative-trial validated methods of analysis of elements and their chemical species in feed. The
terms and definition of the relevant parameters for method validation are included. The performance
requirements and characteristics are provided. This document may serve as a guide:
— to assess the quality of new European Standard methods under validation;
— to review the quality of previous collaborative trials;
— to confirm the extension of the scope of an already published European Standard applied to other
analyte concentrations or matrices; or
— to evaluate the fitness-for-purpose of single-validated methods.
The performance criteria can apply to methods dedicated to the determination of heavy metals, trace
elements, major elements and minerals.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
accuracy
closeness of agreement between a test result and the accepted reference value
[SOURCE: ISO 5725-1, see [12]]
Note 1 to entry: The term accuracy, when applied to a set of test results, involves a combination of random
components and a common systematic error or bias component.
Note 2 to entry: It is assessed by determining trueness and precision.
[SOURCE: 2002/657/EEC, see [13]]
3.2
applicability
scope of the analytical method; description of the analytes, matrices, and concentration ranges (mass
fractions) for which a method of analysis may be used satisfactorily to determine compliance with a
given standard (i.e. CEN, ISO, CODEX)
Note 1 to entry: In addition to a statement of the range of capability of satisfactory performance for each factor,
the statement of applicability (scope) also includes warnings as to known interference by other analytes, or
inapplicability to certain matrices and situations.
3.3
bias
difference between the expectation of the test results (x) and an accepted reference value (x )
ref
[SOURCE: ISO 5725-1, see [12]]
Note 1 to entry: The bias can be expressed in absolute or relative terms (b or b(%), respectively) as:
b xx− (1)
ref
xx−
ref
b(%) × 100 (2)
x
ref
[SOURCE: Eurachem 2014, see [14]]
3.4
inter-laboratory comparison
organisation, performance and evaluation of measurements or tests on the same or similar items by
two or more laboratories in accordance with predetermined conditions
[SOURCE: ISO/IEC 17043:2010, see [15]]
Note 1 to entry: The larger the number of participating laboratories, the greater the confidence that can be
placed in the resulting statistical parameters.
3.4.1
collaborative trials
inter-laboratory comparison aiming at the evaluation of the performance characteristics of a method –
often described as ring-test or ring-trial
[SOURCE: ISO/IEC 17043:2010, see [15]]
Note 1 to entry: It means analysing the same sample by the same method to determine the performance
characteristics of the method.
Note 2 to entry: The study covers random measurement error and laboratory bias.
[SOURCE: 2002/657/EEC, see [13]]
Note 3 to entry: The reported results are used to estimate the performance characteristics of the method, such
as precision. When necessary and possible, other pertinent characteristics such as systematic error and/or
recovery may be reported.
3.4.2
proficiency testing
inter-laboratory comparison aiming at the evaluation of participant performance against pre-
established criteria
[SOURCE: ISO/IEC 17043:2010, see [15]]
Note 1 to entry: The reported results are compared with those from other laboratories or with the known or
assigned reference value, usually with the objective of evaluating or improving laboratory performance.
Note 2 to entry: Proficiency testing means analysing the same sample allowing laboratories to choose their own
methods, provided these methods are used under routine conditions.
[SOURCE: 2002/657/EEC, see [13]]
=
=
3.4.3
reference material characterisation
inter-laboratory comparison aiming at the assignment of values to reference materials and assessment
of their suitability for use in specific test or measurement procedures
[SOURCE: ISO/IEC 17043:2010, see [15]]
3.5
limit of detection
x
LOD
concentration (mass fraction) derived from the smallest measure that can be detected with reasonable
certainty for a given analytical procedure
[SOURCE: ISO 11843, see [16]]
Note 1 to entry: For analytical systems where the validation range does not include or approach it, the detection
limit does not need to be part of a validation.
[SOURCE: IUPAC 2002, see [8]]
Note 2 to entry: The various conceptual approaches to the subject depend on the estimate of precision at or
near zero concentration (mass fraction) under repeatability or reproducibility co
...
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