prEN 17600

Paper and board intended to come into contact with foodstuffs - Determination of the fastness of fluorescent whitened paper and board - Analysis by high-performance liquid chromatography with fluorescence detection

This document describes procedures for the testing of migration of fluorescent whitening agents from paper and board intended to come into contact with foodstuffs. The method is based on liquid chromatography with fluorescence detection for quantification. The document is applicable to four different types of fluorescent whitening agents, diaminostilbene hexasulfonate, diaminostilbene tetrasulfonate, diaminostilbene disulfonate and distyrylbiphenyl.

Papier und Pappe für den Kontakt mit Lebensmitteln - Bestimmung der Farbechtheit von optisch aufgehelltem Papier und Pappe - Analyse durch Hochleistungsflüssigkeitschromatographie mit Fluoreszenzdetektion

Dieses Dokument beschreibt Verfahren zur Prüfung der Migration von optischen Aufhellern aus Papier und Pappe vorgesehen für den Kontakt mit Lebensmitteln. Das Verfahren beruht auf Flüssigkeitschromatographie mit Fluoreszenzdetektion zur Quantifizierung. Das Dokument ist anzuwenden für vier verschiedene Arten von optischen Aufhellern: Diaminostilbenhexasulfonat, Diaminostilbentetrasulfonat, Diaminostilbendisulfonat und Distyrylbiphenyl.

Papiers et cartons destinés à entrer en contact avec des denrées alimentaires - Détermination de la solidité des papiers et cartons blanchis fluorescents - Analyse par chromatographie liquide à haute performance et détection par fluorescence

Le présent document décrit les modes opératoires d'essai de migration des agents d'azurage fluorescents du papier et du carton destinés à entrer en contact avec les denrées alimentaires. La méthode est basée sur la chromatographie liquide et la détection par fluorescence pour la quantification. Le document s’applique à quatre types d'agents d'azurage fluorescents, l’hexasulfonate de diaminostilbène, le tétrasulfonate de diaminostilbène, le disulfonate de diaminostilbène et le distyrylbiphényle.

Papir, karton in lepenka, namenjeni neposrednemu stiku z živili - Ugotavljanje svetlobne obstojnosti papirja, kartona in lepenke, ki vsebujejo optična belila - Analiza s tekočinsko kromatografijo visoke ločljivosti s fluorescenčno detekcijo

General Information

• Status: Not Published
• Publication Date: 18-Dec-2022
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• ICS: 85.060 - Paper and board
• Technical Committee: CEN/TC 172 - Pulp, paper and board
• Drafting Committee: CEN/TC 172/WG 3 - Analytical methods for the assessment of paper and board in contact with foodstuffs
• Current Stage: 4098 - Decision to abandon - Enquiry
• Completion Date: 30-Sep-2022
• Ref Project: oSIST prEN 17600:2020 - Paper and board intended to come into contact with foodstuffs - Determination of the fastness of fluorescent whitened paper and board - Analysis by high-performance liquid chromatography with fluorescence detection

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-2020
Papir, karton in lepenka, namenjeni neposrednemu stiku z živili - Ugotavljanje
svetlobne obstojnosti papirja, kartona in lepenke, ki vsebujejo optična belila -
Analiza s tekočinsko kromatografijo visoke ločljivosti s fluorescenčno detekcijo
Paper and board intended to come into contact with foodstuffs - Determination of the
fastness of fluorescent whitened paper and board - Analysis by high-performance liquid
chromatography with fluorescence detection
Papier und Pappe für den Kontakt mit Lebensmitteln - Bestimmung der Farbechtheit von
optisch aufgehelltem Papier und Pappe - Analyse durch
Hochleistungsflüssigkeitschromatographie mit Fluoreszenzdetektion
Papiers et cartons destinés à entrer en contact avec des denrées alimentaires -
Détermination de la solidité des papiers et cartons blanchis fluorescents - Analyse par
chromatographie liquide à haute performance et détection par fluorescence
Ta slovenski standard je istoveten z: prEN 17600
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
85.060 Papir, karton in lepenka Paper and board
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2020
ICS 67.250; 85.060
English Version
Paper and board intended to come into contact with
foodstuffs - Determination of the fastness of fluorescent
whitened paper and board - Analysis by high-performance
liquid chromatography with fluorescence detection
Papiers et cartons destinés à entrer en contact avec des Papier und Pappe für den Kontakt mit Lebensmitteln -
denrées alimentaires - Détermination de la solidité des Bestimmung der Farbechtheit von optisch
papiers et cartons blanchis fluorescents - Analyse par aufgehelltem Papier und Pappe - Analyse durch
chromatographie liquide à haute performance et Hochleistungsflüssigkeitschromatographie mit
détection par fluorescence Fluoreszenzdetektion
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 172.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17600:2020 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Symbols and abbreviated terms . 4
5 Principle . 4
6 Interferences . 4
7 Test materials and equipment . 5
7.1 General . 5
7.2 Materials . 5
7.3 Apparatus . 5
8 Reagents . 5
9 Preparation of calibration solutions . 6
9.1 Stock solutions of commercially available individual whitening agent at 1g/L . 6
9.2 Individual intermediate solution of commercially available whitening agent at 10 mg/L. 6
9.3 Purity of the stock solution. 6
9.4 Calibration standard solutions of fluorescent whitening agent . 6
10 Sampling . 6
11 Preparation of sample . 6
12 Migration procedure . 6
13 Glass fibre paper extraction . 7
14 Chromatographic analysis procedure . 8
14.1 HPLC conditions . 8
14.2 Calibration . 8
14.3 Analysis of the extracts . 9
14.4 Expression of results . 9
15 Precision data . 10
16 Test report . 10
Annex A (informative) Examples of different types of fluorescent whitening agents . 12

European foreword
This document (prEN 17600:2020) has been prepared by Technical Committee CEN/TC 172 “Pulp,
paper and board”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.

1 Scope
This document describes procedures for the testing of migration of fluorescent whitening agents from
paper and board intended to come into contact with foodstuffs. The method is based on liquid
chromatography with fluorescence detection for quantification. The document is applicable to four
different types of fluorescent whitening agents, diaminostilbene hexasulfonate, diaminostilbene
tetrasulfonate, diaminostilbene disulfonate and distyrylbiphenyl.
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 648, Paper and board intended to come into contact with foodstuffs — Determination of the fastness of
fluorescent whitened paper and board
EN ISO 186, Paper and board — Sampling to determine average quality (ISO 186)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Symbols and abbreviated terms
For the purposes of this document, the following symbols and abbreviated terms apply.
FWA Fluorescent whitening agent
ACN Acetonitrile
DAS Diaminostilbene
5 Principle
A sample is brought into contact with glass fibre papers, which have been saturated with a test fluid and
placed under load for a given time. The test fluids are water, acetic acid 3 %, ethanol 10 % and ethanol
95 %. After short or long contact duration, fluorescent whitening agent are extracted from the glass
fibre and analysed by liquid chromatography-fluorescence detection. The four different types of
fluorescent whitening agent analysed are hexasulfonate, tetrasulfonate, disulfonate and
distyrylbiphenyl without specific separation of the fluorescent whitening agent with the same degree of
sulfonation.
6 Interferences
FWA are extremely sensitive to light. A short contact with UV light can isomerise and destroy these
compounds. Therefore, pay special attention to avoid any contact with light. In order to avoid these
interferences, work in significant darkness or use special light without UV. The flasks shall be protected
with aluminium foil.
7 Test materials and equipment
7.1 General
The used materials shall be free of FWA.
EXAMPLE Common laboratory glassware could be rinsed with water/acetonitrile 50/50 v/v before use.
7.2 Materials
The following materials shall be used.
7.2.1 Pipette of 100 µl to 1 000 µl.
7.2.2 Volumetric brown glass flasks of 50 and 100 ml.
7.2.3 Teflonlined cap brown glass vial, single use.
7.2.4 25 ml brown glass flask.
7.2.5 Whatmann or MN Glassfibre (Under testing at CTP).
7.2.6 Glass plates, 60 mm × 90 mm.
7.2.7 Polyethylene film, uncoloured and transparent.
7.2.8 Mass, 1 kg.
7.3 Apparatus
The usual laboratory apparatus and, in particular, the following, shall be used.
7.3.1 Balance: Analytical of accurately weighting 0,000 1 g.
7.3.2 High Pressure Liquid Chromatograph.
7.3.3 Fluorescence detector.
7.3.4 Column C18: for example ODS, 250 mm × 4,6 mm, particle size 5μm, 120 Å.
7.3.5 Guard column C18: for example Hypersil ODS.
8 Reagents
Use, as far as available, reagents of analytical quality, or better. Verify by blank determinations.
8.1.1 Water for HPLC-Fluorescence detection.
8.1.2 Acetonitrile CAS n° 75-05-8.
8.1.3 Ammonium acetate CAS n° 631-61-8.
8.1.4 Distilled or deionised water.
8.1.5 Acetic acid 3 % m/v.
8.1.6 Ethanol 95 % v/v.
8.1.7 Ethanol 10 % v/v.
8.1.8 Fluorescent whitening agents (FWAs). An example of different types of fluorescent whitening
agents is given in Annex A.
9 Preparation of calibration solutions
9.1 Stock solutions of commercially available individual whitening agent at 1g/L
Prepare stock solutions of individual component by weighing about 100 mg of a whitening agent into
100 ml volumetric flask. Fill the volumetric flask with 50/50 v/v ACN/water, shake to dissolve and
dilute to the mark with the solvent. Protect the flask from light with aluminium foil. Prepare one
solution for each different types of FWA.
Stock solutions shall be stored protected from light at 4 °C and replaced after 1 week.
9.2 Individual intermediate solution of commercially available whitening agent at
10 mg/L
For each of the 4 stock solutions, transfer 1 ml into a 100 ml volumetric flask and dilute to the mark
with the solvent 50/50 v/v ACN/water. Protect the flask with aluminium foil.
The 4 individual intermediate solutions shall be freshly prepared for analysis and stored protected from
light at 4 °C.
9.3 Purity of the stock solution
The amount of active compounds shall be known from the supplier of fluorescent whitening agent.
9.4 Calibration standard solutions of fluorescent whitening agent
Five standard solutions shall be prepared by transferring respectively: 0,125 ml; 0,25 ml; 0,5 ml and
1 ml of the 4 individual intermediate solutions in 50 ml volumetric flasks and 0,1 ml of the 4 individual
intermediate solutions in a 100 ml volumetric flask and adjust the volume with the solvent. The
respective concentrations of the calibration standard solutions are: 10 µg/l; 25 µg/l; 50 µg/l; 100 µg/l
and 200 µg/l of each FWA. At the end of the preparation, the calibration standards shall be protected
from light.
The calibration solutions shall always be freshly prepared and stored
...