ISO 6495-1:2015
(Main)Animal feeding stuffs — Determination of water-soluble chlorides content — Part 1: Titrimetric method
Animal feeding stuffs — Determination of water-soluble chlorides content — Part 1: Titrimetric method
ISO 6495-1:2015 specifies a method for the determination of water-soluble chloride content, expressed as sodium chloride, of animal feeding stuffs. This method is applicable to animal feeding stuffs containing water-soluble chloride content, expressed as sodium chloride, ≥0,05 %.
Aliments des animaux — Détermination de la teneur en chlorures solubles dans l'eau — Partie 1: Méthode titrimétrique
L'ISO 6495-1:2015 spécifie une méthode de détermination de la teneur en chlorures solubles dans l'eau, exprimée en chlorure de sodium, dans les aliments des animaux. Cette méthode est applicable aux aliments des animaux dont la teneur en chlorures solubles dans l'eau, exprimée en chlorure de sodium, est supérieure ou égale à 0,05 %.
Krma - Določevanje v vodi topnih kloridov - 1. del: Titrimetrijska metoda
Ta del standarda ISO 6495 določa metodo za določevanje v vodi topnih kloridov, izraženih kot natrijev klorid, v krmi.
Ta metoda se uporablja za krmo, ki vsebuje v vodi topen klorid, izražen kot natrijev klorid, ≥ 0,05 %.
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INTERNATIONAL ISO
STANDARD 6495-1
First edition
2015-06-15
Animal feeding stuffs —
Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
Aliments des animaux — Détermination de la teneur en chlorures
solubles dans l’eau —
Partie 1: Méthode titrimétrique
Reference number
ISO 6495-1:2015(E)
©
ISO 2015
---------------------- Page: 1 ----------------------
ISO 6495-1:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2015 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 6495-1:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling . 4
7 Preparation of test sample . 4
8 Procedure. 4
8.1 Preparation of test solution . 4
8.1.1 General. 4
8.1.2 Preparation of test solution of sample free from organic matter . 4
8.1.3 Preparation of test solution of sample containing organic matter,
excluding the products listed in 8.1.4 . 4
8.1.4 Cooked feeding stuffs, flax cakes and flour, products rich in flax flour, and
other products rich in mucilage or in colloidal substances . 4
8.2 Titration . 5
8.3 Blank test . 5
9 Expression of results . 6
10 Precision . 6
10.1 Interlaboratory test. 6
10.2 Repeatability . 7
10.3 Reproducibility . 7
11 Test report . 7
Annex A (informative) Results of interlaboratory test . 8
Bibliography . 9
© ISO 2015 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 6495-1:2015(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any
patent rights identified during the development of the document will be in the Introduction and/or on
the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 34, Food Products, Subcommittee SC 10, Animal
feeding stuffs.
This first edition of ISO 6495-1 cancels and replaces ISO 6495:1999, which has been technically revised.
ISO 6495 consists of the following parts, under the general title Animal feeding stuffs — Determination
of water-soluble chloride content:
— Part 1: Titrimetric method
iv © ISO 2015 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 6495-1:2015(E)
Animal feeding stuffs — Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
1 Scope
This part of ISO 6495 specifies a method for the determination of water-soluble chloride content,
expressed as sodium chloride, of animal feeding stuffs.
This method is applicable to animal feeding stuffs containing water-soluble chloride content, expressed
as sodium chloride, ≥0,05 %.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable to its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 6497, Animal feeding stuffs — Sampling
ISO 6498, Animal feeding stuffs — Guidelines for sample preparation
3 Principle
The chloride present in a test portion are dissolved in water. The solution is clarified if the product
contains organic matter. It is then slightly acidified with nitric acid and the chlorides are precipitated
as silver chloride by means of standard volumetric solution of silver nitrate. The excess silver nitrate is
titrated with a standard volumetric solution of ammonium thiocyanate or potassium thiocyanate, by
Volhard’s method.
4 Reagents
Use only reagents of recognized analytical grade.
4.1 Water, complying with at least grade 3 in accordance with ISO 3696.
4.2 Acetone.
4.3 n-Hexane.
4.4 Nitric acid, mass concentration ρ (HNO ) = 1,38 g/ml.
20 3
4.5 Dilute nitric acid, volume fraction ρ(HNO ) = 2 %.
3
Dilute 20 ml nitric acid (4.4) to 1000 ml with water (4.1).
© ISO 2015 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 6495-1:2015(E)
4.6 Potassium chromate solution, mass concentration ρ(K CrO ) = 5 % in water (4.1).
2 4
4.7 Ammonium iron(III) sulfate, saturated solution. Prepare from NH Fe(SO ) ⋅12H O dissolved in
4 4 2 2
water (4.1) until saturation. Approximately 125 g ammonium iron(III) sulfate per 100 ml water is required.
4.8 Activated carbon, free from chloride and not capable of adsorbing chloride.
4.9 Carrez I solution.
Dissolve 10,6 g of potassium hexacyanoferrate(II) trihydrate [K Fe(CN) ⋅3H O] in water (4.1). Dilute to
4 6 2
100 ml with water (4.1).
4.10 Carrez II solution.
Dissolve 21,9 g of zinc acetate dihydrate [Zn(CH COO) ⋅2H O] in water (4.1), and add 3 ml of glacial
3 2 2
acetic acid. Dilute to 100 ml with water (4.1).
4.11 Sodium chloride, standard volumetric solution, c(NaCl) = 0,1 mol/l. The molarity of the standard
volumetric solution shall be known to 0,000 1 mol/l.
Put about 20 g of finely pulverized sodium chloride in a thin layer on watch glass. Dry at about 250 °C
for 1 h to 2 h. Let it cool in a desiccator, accurately weigh 5,8 g, recorded to 0,000 1 g (m), and dissolve in
water (4.1). Dilute to the mark in a 1 000 ml volumetric flask with water (4.1) and mix well.
The concentration of standard sodium chloride solution can be calculated using Formula (1):
m
c = (1)
NaCl
58,44
where
c is the concentration of standard sodium chloride solution, in mol/l;
NaCl
m is the mass of sodium chloride, in grams.
4.12 Silver nitrate, standard volumetric solution, c = 0,1 mol/l.
s
The molarity of the standard volumetric solution should be known to 0,000 1 mol/l, and duplicate
titrations shall agree within ±0,1 ml.
Put about 20 g of finely pulverized silver nitrate in a thin layer on watch glass. Dry at about 80 °C for 2 h
to 3 h. Let it cool in a desiccator, weigh about 17,0 g and dissolve in water (4.1). Dilute to the mark in a
1 000 ml volumetric flask with water (4.1) and mix well.
Pipette 20 ml of standard sodium chloride solution (4.11) into a 200 ml conical flask. Add 1 ml of
potassium chromate solution (4.6) and titrate while shaking vigorously with standard silver
...
SLOVENSKI STANDARD
SIST ISO 6495-1:2018
01-oktober-2018
1DGRPHãþD
SIST ISO 6495:2000
.UPD'RORþHYDQMHYYRGLWRSQLKNORULGRYGHO 7LWULPHWULMVNDPHWRGD
Animal feeding stuffs -- Determination of water-soluble chlorides content -- Part 1:
Titrimetric method
Aliments des animaux -- Détermination de la teneur en chlorures solubles dans l'eau --
Partie 1: Méthode titrimétrique
Ta slovenski standard je istoveten z: ISO 6495-1:2015
ICS:
65.120 Krmila Animal feeding stuffs
SIST ISO 6495-1:2018 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 6495-1:2018
---------------------- Page: 2 ----------------------
SIST ISO 6495-1:2018
INTERNATIONAL ISO
STANDARD 6495-1
First edition
2015-06-15
Animal feeding stuffs —
Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
Aliments des animaux — Détermination de la teneur en chlorures
solubles dans l’eau —
Partie 1: Méthode titrimétrique
Reference number
ISO 6495-1:2015(E)
©
ISO 2015
---------------------- Page: 3 ----------------------
SIST ISO 6495-1:2018
ISO 6495-1:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2015 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 6495-1:2018
ISO 6495-1:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling . 4
7 Preparation of test sample . 4
8 Procedure. 4
8.1 Preparation of test solution . 4
8.1.1 General. 4
8.1.2 Preparation of test solution of sample free from organic matter . 4
8.1.3 Preparation of test solution of sample containing organic matter,
excluding the products listed in 8.1.4 . 4
8.1.4 Cooked feeding stuffs, flax cakes and flour, products rich in flax flour, and
other products rich in mucilage or in colloidal substances . 4
8.2 Titration . 5
8.3 Blank test . 5
9 Expression of results . 6
10 Precision . 6
10.1 Interlaboratory test. 6
10.2 Repeatability . 7
10.3 Reproducibility . 7
11 Test report . 7
Annex A (informative) Results of interlaboratory test . 8
Bibliography . 9
© ISO 2015 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 6495-1:2018
ISO 6495-1:2015(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any
patent rights identified during the development of the document will be in the Introduction and/or on
the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 34, Food Products, Subcommittee SC 10, Animal
feeding stuffs.
This first edition of ISO 6495-1 cancels and replaces ISO 6495:1999, which has been technically revised.
ISO 6495 consists of the following parts, under the general title Animal feeding stuffs — Determination
of water-soluble chloride content:
— Part 1: Titrimetric method
iv © ISO 2015 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 6495-1:2018
INTERNATIONAL STANDARD ISO 6495-1:2015(E)
Animal feeding stuffs — Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
1 Scope
This part of ISO 6495 specifies a method for the determination of water-soluble chloride content,
expressed as sodium chloride, of animal feeding stuffs.
This method is applicable to animal feeding stuffs containing water-soluble chloride content, expressed
as sodium chloride, ≥0,05 %.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable to its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 6497, Animal feeding stuffs — Sampling
ISO 6498, Animal feeding stuffs — Guidelines for sample preparation
3 Principle
The chloride present in a test portion are dissolved in water. The solution is clarified if the product
contains organic matter. It is then slightly acidified with nitric acid and the chlorides are precipitated
as silver chloride by means of standard volumetric solution of silver nitrate. The excess silver nitrate is
titrated with a standard volumetric solution of ammonium thiocyanate or potassium thiocyanate, by
Volhard’s method.
4 Reagents
Use only reagents of recognized analytical grade.
4.1 Water, complying with at least grade 3 in accordance with ISO 3696.
4.2 Acetone.
4.3 n-Hexane.
4.4 Nitric acid, mass concentration ρ (HNO ) = 1,38 g/ml.
20 3
4.5 Dilute nitric acid, volume fraction ρ(HNO ) = 2 %.
3
Dilute 20 ml nitric acid (4.4) to 1000 ml with water (4.1).
© ISO 2015 – All rights reserved 1
---------------------- Page: 7 ----------------------
SIST ISO 6495-1:2018
ISO 6495-1:2015(E)
4.6 Potassium chromate solution, mass concentration ρ(K CrO ) = 5 % in water (4.1).
2 4
4.7 Ammonium iron(III) sulfate, saturated solution. Prepare from NH Fe(SO ) ⋅12H O dissolved in
4 4 2 2
water (4.1) until saturation. Approximately 125 g ammonium iron(III) sulfate per 100 ml water is required.
4.8 Activated carbon, free from chloride and not capable of adsorbing chloride.
4.9 Carrez I solution.
Dissolve 10,6 g of potassium hexacyanoferrate(II) trihydrate [K Fe(CN) ⋅3H O] in water (4.1). Dilute to
4 6 2
100 ml with water (4.1).
4.10 Carrez II solution.
Dissolve 21,9 g of zinc acetate dihydrate [Zn(CH COO) ⋅2H O] in water (4.1), and add 3 ml of glacial
3 2 2
acetic acid. Dilute to 100 ml with water (4.1).
4.11 Sodium chloride, standard volumetric solution, c(NaCl) = 0,1 mol/l. The molarity of the standard
volumetric solution shall be known to 0,000 1 mol/l.
Put about 20 g of finely pulverized sodium chloride in a thin layer on watch glass. Dry at about 250 °C
for 1 h to 2 h. Let it cool in a desiccator, accurately weigh 5,8 g, recorded to 0,000 1 g (m), and dissolve in
water (4.1). Dilute to the mark in a 1 000 ml volumetric flask with water (4.1) and mix well.
The concentration of standard sodium chloride solution can be calculated using Formula (1):
m
c = (1)
NaCl
58,44
where
c is the concentration of standard sodium chloride solution, in mol/l;
NaCl
m is the mass of sodium chloride, in grams.
4.12 Silver nitrate, standard volumetric solution, c = 0,1 mol/l.
s
The molarity of the standard volumetric solution should be known to 0,000 1 mol/l, and duplicate
titrations shall agree within ±0,1 ml.
Put about 20 g of finely pulverize
...
NORME ISO
INTERNATIONALE 6495-1
Première édition
2015-06-15
Aliments des animaux —
Détermination de la teneur en
chlorures solubles dans l’eau —
Partie 1:
Méthode titrimétrique
Animal feeding stuffs — Determination of water-soluble chlorides
content —
Part 1: Titrimetric method
Numéro de référence
ISO 6495-1:2015(F)
©
ISO 2015
---------------------- Page: 1 ----------------------
ISO 6495-1:2015(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2015
Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée
sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie, l’affichage sur
l’internet ou sur un Intranet, sans autorisation écrite préalable. Les demandes d’autorisation peuvent être adressées à l’ISO à
l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Publié en Suisse
ii © ISO 2015 – Tous droits réservés
---------------------- Page: 2 ----------------------
ISO 6495-1:2015(F)
Sommaire Page
Avant-propos .iv
1 Domaine d’application . 1
2 Références normatives . 1
3 Principe . 1
4 Réactifs . 1
5 Appareillage . 3
6 Échantillonnage . 4
7 Préparation de l’échantillon pour essai . 4
8 Mode opératoire. 4
8.1 Préparation de la solution d’essai . 4
8.1.1 Généralités . 4
8.1.2 Préparation de la solution d’essai d’échantillons exempts de
matières organiques . 4
8.1.3 Préparation de la solution d’essai d’échantillons contenant des matières
organiques, à l’exception des produits mentionnés en 8.1.4 . 4
8.1.4 Aliments cuits, tourteaux et farine de lin, produits riches en farine de lin
et autres produits riches en mucilages ou en substances colloïdales . 4
8.2 Titrage . 5
8.3 Essai à blanc . 5
9 Expression des résultats. 6
10 Fidélité . 6
10.1 Essai interlaboratoires . 6
10.2 Répétabilité . 6
10.3 Reproductibilité . 7
11 Rapport d’essai . 7
Annexe A (informative) Résultats de l’essai interlaboratoires . 8
Bibliographie . 9
© ISO 2015 – Tous droits réservés iii
---------------------- Page: 3 ----------------------
ISO 6495-1:2015(F)
Avant-propos
L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes
nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est
en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.
L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui concerne
la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www.
iso.org/directives).
L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de
droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant les
références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de l’élaboration
du document sont indiqués dans l’Introduction et/ou dans la liste des déclarations de brevets reçues par
l’ISO (voir www.iso.org/brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données pour
information, par souci de commodité à l’intention des utilisateurs et ne sauraient constituer un engagement.
Pour une explication de la signification des termes et expressions spécifiques de l’ISO liés à l’évaluation de
la conformité, ou pour toute information au sujet de l’adhésion de l’ISO aux principes de l’OMC concernant
les obstacles techniques au commerce (OTC), voir le lien suivant: Avant-propos — Informations
supplémentaires.
Le comité chargé de l’élaboration du présent document est l’ISO/TC 34, Produits alimentaires, sous-
comité SC 10, Aliments des animaux.
Cette première édition de l’ISO 6495-1 annule et remplace l’ISO 6495:1999, qui a fait l’objet d’une
révision technique.
L’ISO 6495 comprend les parties suivantes, présentées sous le titre général Aliments des animaux —
Détermination de la teneur en chlorures solubles dans l’eau:
— Partie 1: Méthode titrimétrique
iv © ISO 2015 – Tous droits réservés
---------------------- Page: 4 ----------------------
NORME INTERNATIONALE ISO 6495-1:2015(F)
Aliments des animaux — Détermination de la teneur en
chlorures solubles dans l’eau —
Partie 1:
Méthode titrimétrique
1 Domaine d’application
La présente partie de l’ISO 6495 spécifie une méthode de détermination de la teneur en chlorures
solubles dans l’eau, exprimée en chlorure de sodium, dans les aliments des animaux.
Cette méthode est applicable aux aliments des animaux dont la teneur en chlorures solubles dans l’eau,
exprimée en chlorure de sodium, est supérieure ou égale à 0,05 %.
2 Références normatives
Les documents ci-après, dans leur intégralité ou non, sont des références normatives indispensables à
l’application du présent document. Pour les références datées, seule l’édition citée s’applique. Pour les
références non datées, la dernière édition du document de référence s’applique (y compris les éventuels
amendements).
ISO 3696, Eau pour laboratoire à usage analytique — Spécification et méthodes d’essai
ISO 6497, Aliments des animaux — Échantillonnage
ISO 6498, Aliments des animaux —Lignes directrices pour la préparation des échantillons
3 Principe
Mise en solution dans l’eau des chlorures présents dans une prise d’essai. Clarification de la solution si
le produit contient des matières organiques. Légère acidification par l’acide nitrique et précipitation des
chlorures sous forme de chlorure d’argent à l’aide d’une solution titrée de nitrate d’argent. Titrage de
l’excès de nitrate d’argent par une solution titrée de thiocyanate d’ammonium ou de potassium, selon la
méthode de Volhard.
4 Réactifs
Utiliser uniquement des réactifs de qualité analytique reconnue.
4.1 Eau, de qualité 3 au minimum, conformément à l’ISO 3696.
4.2 Acétone.
4.3 n-Hexane.
4.4 Acide nitrique, concentration massique ρ (HNO ) = 1,38 g/ml.
20 3
4.5 Acide nitrique dilué, fraction volumique ρ(HNO ) = 2 %.
3
Diluer 20 ml d’acide nitrique (4.4) à 1 000 ml avec de l’eau (4.1).
© ISO 2015 – Tous droits réservés 1
---------------------- Page: 5 ----------------------
ISO 6495-1:2015(F)
4.6 Solution de chromate de potassium, concentration massique ρ(K CrO ) = 5 % dans l’eau (4.1).
2 4
4.7 Sulfate d’ammonium et de fer(III), solution saturée. Préparer à partir de NH Fe(SO ) ⋅12H O
4 4 2 2
dissous dans de l’eau (4.1) jusqu’à saturation. Environ 125 g de sulfate d’ammonium et de fer(III) pour
100 ml d’eau sont requis.
4.8 Charbon actif, exempt de chlorures et ne pouvant en adsorber.
4.9 Solution de Carrez I.
Dissoudre 10,6 g d’hexacyanoferrate de potassium(II) trihydraté [K Fe(CN) ⋅3H O] dans de l’eau (4.1).
4 6 2
Compléter à 100 ml avec de l’eau (4.1).
4.10 Solution de Carrez II.
Dissoudre 21,9 g d’acétate de zinc dihydraté [Zn(CH COO) ⋅2H O] dans de l’eau (4.1), et ajouter 3 ml
3 2 2
d’acide acétique glacial. Compléter à 100 ml avec de l’eau (4.1).
4.11 Chlorure de sodium, solution titrée, c(NaCl) = 0,1 mol/l. La molarité de la solution titrée doit être
connue à 0,000 1 mol/l près.
Étaler en couche mince, sur un verre de montre, environ 20 g de chlorure de sodium finement pulvérisé.
Sécher à 250 °C environ pendant 1 h à 2 h. Laisser refroidir dans un dessiccateur, peser exactement
5,8 g, consignés à 0,000 1 g (m) près, et dissoudre dans de l’eau (4.1). Compléter au volume dans une fiole
jaugée de 1 000 ml avec de l’eau (4.1) et bien mélanger.
La concentration de la solution titrée de chlorure de sodium peut être calculée à l’aide de la Formule (1):
m
c = (1)
NaCl
58,44
où
c est la concentration de la solution titrée de chlorure de sodium, en mol/l;
NaCl
m est la masse de chlorure de sodium, en grammes.
4.12 Nitrate d’argent, solution titrée, c = 0,1 mol/l.
s
Il convient que la molarité de la solution titrée soit connue à 0,000 1 mol/l près, et les titrages en double
doivent s’inscrire dans les limites de ± 0,1 ml.
Étaler en couche mince, sur un verre de montre, environ 20 g de nitrate d’argent finement pulvérisé.
Sécher à 80 °C environ pendant 2 h à 3 h. Laisser refroidir dans un dessiccateur, peser environ 17,0 g et
dissoudre dans de l’eau (4.1). Compléter au volume dans une fiole jaugée de 1 000 ml avec de l’eau (4.1)
et bien mélanger.
À l’aide d’une pipette, introduire 20 ml de solution titrée de chlorure de sodium (4.11) dans une fiole
conique de 200 ml. Ajouter 1 ml de solution de chromate de potassium (4.6) et titrer tout en agitant
vigoureusement avec la solution titrée de nitrate d’argent (4.12) jusqu’à obtention d’une couleur rouge-
brun persistant pendant au moins 30 s.
2 © ISO 2015 – Tous droits réservés
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ISO 6495-1:2015(F)
La concentration de la solution titrée de nitrate d’argent peut êtr
...
SLOVENSKI STANDARD
oSIST ISO 6495-1:2018
01-september-2018
.UPD'RORþHYDQMHYYRGLWRSQLKNORULGRYGHO 7LWULPHWULMVNDPHWRGD
Animal feeding stuffs -- Determination of water-soluble chlorides content -- Part 1:
Titrimetric method
Aliments des animaux -- Détermination de la teneur en chlorures solubles dans l'eau --
Partie 1: Méthode titrimétrique
Ta slovenski standard je istoveten z: ISO 6495-1:2015
ICS:
65.120 Krmila Animal feeding stuffs
oSIST ISO 6495-1:2018 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST ISO 6495-1:2018
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oSIST ISO 6495-1:2018
INTERNATIONAL ISO
STANDARD 6495-1
First edition
2015-06-15
Animal feeding stuffs —
Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
Aliments des animaux — Détermination de la teneur en chlorures
solubles dans l’eau —
Partie 1: Méthode titrimétrique
Reference number
ISO 6495-1:2015(E)
©
ISO 2015
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oSIST ISO 6495-1:2018
ISO 6495-1:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
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Tel. + 41 22 749 01 11
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Published in Switzerland
ii © ISO 2015 – All rights reserved
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oSIST ISO 6495-1:2018
ISO 6495-1:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling . 4
7 Preparation of test sample . 4
8 Procedure. 4
8.1 Preparation of test solution . 4
8.1.1 General. 4
8.1.2 Preparation of test solution of sample free from organic matter . 4
8.1.3 Preparation of test solution of sample containing organic matter,
excluding the products listed in 8.1.4 . 4
8.1.4 Cooked feeding stuffs, flax cakes and flour, products rich in flax flour, and
other products rich in mucilage or in colloidal substances . 4
8.2 Titration . 5
8.3 Blank test . 5
9 Expression of results . 6
10 Precision . 6
10.1 Interlaboratory test. 6
10.2 Repeatability . 7
10.3 Reproducibility . 7
11 Test report . 7
Annex A (informative) Results of interlaboratory test . 8
Bibliography . 9
© ISO 2015 – All rights reserved iii
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oSIST ISO 6495-1:2018
ISO 6495-1:2015(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any
patent rights identified during the development of the document will be in the Introduction and/or on
the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 34, Food Products, Subcommittee SC 10, Animal
feeding stuffs.
This first edition of ISO 6495-1 cancels and replaces ISO 6495:1999, which has been technically revised.
ISO 6495 consists of the following parts, under the general title Animal feeding stuffs — Determination
of water-soluble chloride content:
— Part 1: Titrimetric method
iv © ISO 2015 – All rights reserved
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oSIST ISO 6495-1:2018
INTERNATIONAL STANDARD ISO 6495-1:2015(E)
Animal feeding stuffs — Determination of water-soluble
chlorides content —
Part 1:
Titrimetric method
1 Scope
This part of ISO 6495 specifies a method for the determination of water-soluble chloride content,
expressed as sodium chloride, of animal feeding stuffs.
This method is applicable to animal feeding stuffs containing water-soluble chloride content, expressed
as sodium chloride, ≥0,05 %.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable to its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 6497, Animal feeding stuffs — Sampling
ISO 6498, Animal feeding stuffs — Guidelines for sample preparation
3 Principle
The chloride present in a test portion are dissolved in water. The solution is clarified if the product
contains organic matter. It is then slightly acidified with nitric acid and the chlorides are precipitated
as silver chloride by means of standard volumetric solution of silver nitrate. The excess silver nitrate is
titrated with a standard volumetric solution of ammonium thiocyanate or potassium thiocyanate, by
Volhard’s method.
4 Reagents
Use only reagents of recognized analytical grade.
4.1 Water, complying with at least grade 3 in accordance with ISO 3696.
4.2 Acetone.
4.3 n-Hexane.
4.4 Nitric acid, mass concentration ρ (HNO ) = 1,38 g/ml.
20 3
4.5 Dilute nitric acid, volume fraction ρ(HNO ) = 2 %.
3
Dilute 20 ml nitric acid (4.4) to 1000 ml with water (4.1).
© ISO 2015 – All rights reserved 1
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oSIST ISO 6495-1:2018
ISO 6495-1:2015(E)
4.6 Potassium chromate solution, mass concentration ρ(K CrO ) = 5 % in water (4.1).
2 4
4.7 Ammonium iron(III) sulfate, saturated solution. Prepare from NH Fe(SO ) ⋅12H O dissolved in
4 4 2 2
water (4.1) until saturation. Approximately 125 g ammonium iron(III) sulfate per 100 ml water is required.
4.8 Activated carbon, free from chloride and not capable of adsorbing chloride.
4.9 Carrez I solution.
Dissolve 10,6 g of potassium hexacyanoferrate(II) trihydrate [K Fe(CN) ⋅3H O] in water (4.1). Dilute to
4 6 2
100 ml with water (4.1).
4.10 Carrez II solution.
Dissolve 21,9 g of zinc acetate dihydrate [Zn(CH COO) ⋅2H O] in water (4.1), and add 3 ml of glacial
3 2 2
acetic acid. Dilute to 100 ml with water (4.1).
4.11 Sodium chloride, standard volumetric solution, c(NaCl) = 0,1 mol/l. The molarity of the standard
volumetric solution shall be known to 0,000 1 mol/l.
Put about 20 g of finely pulverized sodium chloride in a thin layer on watch glass. Dry at about 250 °C
for 1 h to 2 h. Let it cool in a desiccator, accurately weigh 5,8 g, recorded to 0,000 1 g (m), and dissolve in
water (4.1). Dilute to the mark in a 1 000 ml volumetric flask with water (4.1) and mix well.
The concentration of standard sodium chloride solution can be calculated using Formula (1):
m
c = (1)
NaCl
58,44
where
c is the concentration of standard sodium chloride solution, in mol/l;
NaCl
m is the mass of sodium chloride, in grams.
4.12 Silver nitrate, standard volumetric solution, c = 0,1 mol/l.
s
The molarity of the standard volumetric solution should be known to 0,000 1 mol/l, and duplicate
titrations shall agree within ±0,1 ml.
Put about 20 g of finely pulverized silver nit
...
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