Pulp, paper and paperboard - Determination of anthraquinone in extracts from pulp, paper and paperboard

This document specifies an analytical test method for the determination of anthraquinone (see Table 1) in water and 95 % ethanol extracts of pulp, paper and board materials and articles intended to come into contact with foodstuffs using a gas chromatograph coupled to a mass spectrometer (GC-MS). Moreover, acetone extracts of modified polyphenylene oxide (MPPO) that, according to EN 14338, can be used as a simulant to assess the possible transfer/migration of substances from paper and board into dry, non-fatty foodstuffs can be analysed with the method presented here.
This method can be applied to determine anthraquinone in concentrations ranging from 2 μg/l to 40 μg/l in the water and solvent extracts, corresponding to 0,05 mg/kg to 1 mg/kg pulp, paper and board or, respectively, 0,1 μg/dm2 to 2 μg/dm2 in the case of migration tests with MPPO. The measurement range can be lowered by enriching anthraquinone from the water and solvent extracts.

Faserstoff, Papier und Karton - Bestimmung von Anthrachinon in Faserstoff-, Papier- und Kartonextrakten

Dieses Dokument legt ein Analyseverfahren zur Bestimmung von Anthrachinon (siehe Tabelle 1) in Wasser und 95%igen Ethanolextrakten von Faserstoff , Papier  und Kartonmaterialien und  gegenständen, die dazu bestimmt sind, mit Lebensmitteln in Berührung zu kommen, unter Verwendung eines Gaschromatographen, der mit einem Massenspektrometer gekoppelt ist (GC MS), fest. Darüber hinaus können Aceton Extrakte von modifizierten Polyphenyloxiden (MPPO, en: modified polyphenylene oxide), die nach EN 14338 als Simulanz verwendet werden können, um den möglichen Übergang/die mögliche Migration von Substanzen aus Papier und Karton in trockene, fettfreie Lebensmittel zu beurteilen, mit dem dargestellten Verfahren analysiert werden.
Dieses Verfahren kann angewendet werden, um Anthrachinon in Konzentrationen von 2 µg/l bis 40 µg/l im Wasser beziehungsweise den Lösemittelextrakten, entsprechend 0,05 mg/kg bis 1 mg/kg Faserstoff, Papier und Karton, beziehungsweise 0,1 μg/dm2 bis 2 μg/dm2 im Fall von Migrationsversuchen mit MPPO, zu bestimmen. Der Messbereich kann durch Anreichern von Anthrachinon aus dem Wasser und den Lösemittelextrakten gesenkt werden.
[Tabelle 1]

Pâte, papier et carton - Détermination d'anthraquinone dans des extraits de pâte, papier et carton

Le présent document spécifie une méthode d’essai analytique pour la détermination de l’anthraquinone (voir Tableau 1) dans des extraits à l’eau et l’éthanol à 95 % de matériaux et articles destinés à entrer en contact avec les denrées alimentaires sous forme de pâte, papier et carton en utilisant un chromatographe en phase gazeuse couplé à un spectromètre de masse (CG-SM). De plus, des extraits à l’acétone d’oxyde de polyphénylène modifié (MPPO) qui, conformément à l’EN 14338, peuvent être utilisés comme solvant simulant pour évaluer le transfert/la migration possible de substances issues du papier et du carton dans des denrées alimentaires sèches, non grasses, peuvent être analysés par la méthode présentée ici.
Cette méthode peut être appliquée pour déterminer l’anthraquinone dans des concentrations se situant dans la plage de 2 μg/l à 40 μg/l dans les extraits aqueux et de solvant, correspondant à 0,05 mg/kg à 1 mg/kg de pâte, de papier et de carton ou, respectivement, 0,1 μg/dm2 à 2 μg/dm2 dans le cas d’essais de migration avec du MPPO. La plage de mesurage peut être abaissée en enrichissant l’anthraquinone à partir des extraits aqueux et de solvant.

Vlaknine, papir, karton in lepenka - Določanje koncentracije antrakinona v ekstraktih vlaknin, papirja, kartona in lepenke

General Information

Status
Published
Publication Date
22-Jun-2021
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
23-Jun-2021
Due Date
21-Jun-2021
Completion Date
23-Jun-2021

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17630:2021
01-september-2021
Vlaknine, papir, karton in lepenka - Določanje koncentracije antrakinona v
ekstraktih vlaknin, papirja, kartona in lepenke
Pulp, paper and paperboard - Determination of anthraquinone in extracts from pulp,
paper and paperboard
Faserstoff, Papier und Karton - Bestimmung von Anthrachinon in Faserstoff-, Papier- und
Kartonextraten
Pâte, papier et carton - Détermination d'anthraquinone dans des extraits de pâte, papier
et carton
Ta slovenski standard je istoveten z: CEN/TS 17630:2021
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
85.040 Vlaknine Pulps
85.060 Papir, karton in lepenka Paper and board
SIST-TS CEN/TS 17630:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 17630:2021

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SIST-TS CEN/TS 17630:2021


CEN/TS 17630
TECHNICAL SPECIFICATION

SPÉCIFICATION TECHNIQUE

June 2021
TECHNISCHE SPEZIFIKATION
ICS 67.250; 85.060
English Version

Pulp, paper and paperboard - Determination of
anthraquinone in extracts from pulp, paper and
paperboard
Pâte, papier et carton - Détermination d'anthraquinone Faserstoff, Papier und Karton - Bestimmung von
dans des extraits de pâte, papier et carton Anthrachinon in Faserstoff-, Papier- und
Kartonextraten
This Technical Specification (CEN/TS) was approved by CEN on 9 May 2021 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, Republic of North Macedonia, 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
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17630:2021 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17630:2021
CEN/TS 17630:2021 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 5
4 Principle . 5
5 Materials . 5
6 Apparatus . 5
7 Reagents . 6
8 Sampling . 7
9 Preparation of the analysis solutions from water extracts . 7
10 Preparation of the analysis solutions from 95 % ethanol extracts. 8
11 Preparation of the analysis solutions from MPPO . 8
12 Procedure. 8
13 Expression of results . 10
14 Test report . 11
15 Precision data . 11

2

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17630:2021
CEN/TS 17630:2021 (E)
European foreword
This document (CEN/TS 17630:2021) has been prepared by Technical Committee CEN/TC 172 “Pulp,
paper and board”, 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 shall not be held responsible for identifying any or all such patent rights.
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, 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 the United
Kingdom.
3

---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 17630:2021
CEN/TS 17630:2021 (E)
1 Scope
This document specifies an analytical test method for the determination of anthraquinone (see Table 1)
in water and 95 % ethanol extracts of pulp, paper and board materials and articles intended to come into
contact with foodstuffs using a gas chromatograph coupled to a mass spectrometer (GC-MS). Moreover,
acetone extracts of modified polyphenylene oxide (MPPO) that, according to EN 14338, can be used as a
simulant to assess the possible transfer/migration of substances from paper and board into dry, non-
fatty foodstuffs can be analysed with the method presented here.
This method can be applied to determine anthraquinone in concentrations ranging from 2 µg/l to 40 µg/l
in the water and solvent extracts, corresponding to 0,05 mg/kg to 1 mg/kg pulp, paper and board or,
2 2
respectively, 0,1 μg/dm to 2 μg/dm in the case of migration tests with MPPO. The measurement range
can be lowered by enriching anthraquinone from the water and solvent extracts.
Table 1 — Anthraquinone
Name Abbreviation Formula CAS N° Structure
C H O
Anthraquinone AQ 84-65-1
14 8 2

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 645, Paper and board intended to come into contact with foodstuffs — Preparation of a cold water
extract
EN 647, Paper and board intended to come into contact with foodstuffs — Preparation of a hot water
extract
EN 14338, Paper and board intended to come into contact with foodstuffs — Conditions for determination
of migration from paper and board using modified polyphenylene oxide (MPPO) as a simulant
EN 15519, Paper and board intended to come into contact with foodstuffs — Preparation of an organic
solvent extract
EN 27213, Pulps — Sampling for testing (ISO 7213)
EN ISO 186, Paper and board — Sampling to determine average quality (ISO 186)
EN ISO 536, Paper and board — Determination of grammage (ISO 536)
EN ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method
(ISO 638)
ISO 3696, Water for analytical laboratory use — Specification and test methods
4

---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17630:2021
CEN/TS 17630:2021 (E)
3 Terms and definitions
No terms and definitions are listed in this document.
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/ui
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
4.1 General
Anthraquinone is extracted from pulp, paper and board with water and/or 95 % ethanol according to
EN 645, EN 647 and/or EN 15519, and with acetone from MPPO which was brought into contact with the
materials as a simulant for dry, non-fatty foodstuffs according to EN 14338. GC-MS is used to determine
the anthraquinone content in the prepared extracts.
4.2 Interferences
Matrix related interferences can occur. In these cases, the quantification of anthraquinone may be
performed by using one of the qualifier ions (12.1.2) or by standard addition.
5 Materials
5.1 Pasteur pipettes.
5.2 Piston pipettes with a capacity adjustable from 3 µl to 25 µl, 20 µl to 50 µl, 50 µl to 250 µl and
100 µl to 1 000 µl.
5.3 Volumetric pipettes with a capacity of 2 ml, 5 ml and 10 ml.
5.4 Volumetric flasks with a capacity of 5 ml, 10 ml, 25 ml and 100 ml.
5.5 Pear shaped flasks with a capacity adapted to the volume of the extract, e.g. 25 ml.
5.6 Glass flasks with polytetrafluoroethylene (PTFE) lined screw caps with a capacity adapted to
the volume of the extract, e.g. 25 ml.
5.7 Disposable screw thread glass vials with a capacity of 1,5 ml and the corresponding
polypropylene (PP) caps with silicone/PTFE gaskets.
6 Apparatus
6.1 Balance capable of accurately weighing 0,000 1 g.
6.2 Rotary evaporator.
6.3 Gas chromatograph coupled to a mass spectrometer (GC-MS).
5

---------------------- Page: 7 ----------------------
SIST-TS CEN/TS 17630:2021
CEN/TS 17630:2021 (E)
7 Reagents
All reagents should be of analytical grade or better.
7.1 Water, grade 1 according to ISO 3696.
7.2 Ethanol, a volume fraction of 95 %.
7.3 Toluene, ≥ 99 %.
7.4 Acetone, ≥ 99 %.
7.5 Solutions of the internal standard
7.5.1 Anthracene-d10 (internal standard), CAS N° 1719-06-8.
Commercial ready-to-use solutions at 10 mg/l in cyclohexene are available.
7.5.2 Intermediate soluti
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17630:2021
01-marec-2021
Vlaknine, papir, karton in lepenka - Ugotavljanje koncentracije antrakinona v
ekstraktih vlaknin, papirja, kartona in lepenke
Pulp, paper and paperboard - Determination of anthraquinone in extracts from pulp,
paper and paperboard
Faserstoff, Papier und Karton - Bestimmung von Anthrachinon in Faserstoff-, Papier- und
Kartonextraten
Pâte, papier et carton - Détermination d'anthraquinone dans des extraits de pâte, papier
et carton
Ta slovenski standard je istoveten z: FprCEN/TS 17630
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
85.040 Vlaknine Pulps
85.060 Papir, karton in lepenka Paper and board
kSIST-TS FprCEN/TS 17630:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17630:2021

---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17630:2021


FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17630
SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION

January 2021
ICS 67.250; 85.060
English Version

Pulp, paper and paperboard - Determination of
anthraquinone in extracts from pulp, paper and
paperboard
Pâte, papier et carton - Détermination d'anthraquinone Faserstoff, Papier und Karton - Bestimmung von
dans des extraits de pâte, papier et carton Anthrachinon in Faserstoff-, Papier- und
Kartonextraten


This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee
CEN/TC 172.

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 Technical Specification. It is distributed for review and comments. It is subject to change
without notice and shall not be referred to as a Technical Specification.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17630:2021 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17630:2021
FprCEN/TS 17630:2021 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 5
4 Principle . 5
5 Materials . 5
6 Apparatus . 5
7 Reagents . 6
8 Sampling . 7
9 Preparation of the analysis solutions from water extracts . 7
10 Preparation of the analysis solutions from 95 % ethanol extracts. 7
11 Preparation of the analysis solutions from MPPO . 8
12 Procedure. 8
13 Expression of results . 9
14 Test report . 10
15 Precision data . 10

2

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17630:2021
FprCEN/TS 17630:2021 (E)

European foreword
This document (FprCEN/TS 17630:2021) 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 Vote on TS.

3

---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17630:2021
FprCEN/TS 17630:2021 (E)
1 Scope
This document specifies an analytical test method for the determination of anthraquinone (see Table 1)
in water and 95 % ethanol extracts of pulp, paper and board materials and articles intended to come into
contact with foodstuffs using a gas chromatograph coupled to a mass spectrometer (GC-MS). Moreover,
acetone extracts of modified polyphenylene oxide (MPPO) that, according to EN 14338, can be used as a
simulant to assess the possible transfer/migration of substances from paper and board into dry, non-
fatty foodstuffs can be analysed with the method presented here.
This method can be applied to determine anthraquinone in concentrations ranging from 2 µg/l to 40 µg/l
in the water and solvent extracts, corresponding to 0,05 mg/kg to 1 mg/kg pulp, paper and board or,
2 2
respectively, 0,1 μg/dm to 2 μg/dm in the case of migration tests with MPPO. The measurement range
can be lowered by enriching anthraquinone from the water and solvent extracts.
Table 1 — Anthraquinone
Name Abbreviation Formula CAS N° Structure
C H O
Anthraquinone AQ 84-65-1
14 8 2

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 645, Paper and board intended to come into contact with foodstuffs — Preparation of a cold water
extract
EN 647, Paper and board intended to come into contact with foodstuffs — Preparation of a hot water
extract
EN 14338, Paper and board intended to come into contact with foodstuffs — Conditions for determination
of migration from paper and board using modified polyphenylene oxide (MPPO) as a simulant
EN 15519, Paper and board intended to come into contact with foodstuffs — Preparation of an organic
solvent extract
EN 27213, Pulps — Sampling for testing (ISO 7213)
EN ISO 186, Paper and board — Sampling to determine average quality (ISO 186)
EN ISO 536, Paper and board — Determination of grammage (ISO 536)
EN ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method (ISO
638)
ISO 3696, Water for analytical laboratory use — Specification and test methods
4

---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17630:2021
FprCEN/TS 17630:2021 (E)

3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/ui
4 Principle
4.1 General
Anthraquinone is extracted from pulp, paper and board with water and/or 95 % ethanol according to
EN 645, EN 647 and/or EN 15519, and with acetone from MPPO which was brought into contact with the
materials as a simulant for dry, non-fatty foodstuffs according to EN 14338. GC-MS is used to determine
the anthraquinone content in the prepared extracts.
4.2 Interferences
Matrix related interferences can occur. In these cases, the quantification of anthraquinone may be
performed by using one of the qualifier ions (12.1.2) or by standard addition.
5 Materials
5.1 Pasteur pipettes.
5.2 Piston pipettes with a capacity adjustable from 3 µl to 25 µl, 20 µl to 50 µl, 50 µl to 250 µl and
100 µl to 1 000 µl.
5.3 Volumetric pipettes with a capacity of 2 ml, 5 ml and 10 ml.
5.4 Volumetric flasks with a capacity of 5 ml, 10 ml, 25 ml and 100 ml.
5.5 Pear shaped flasks with a capacity adapted to the volume of the extract, e.g. 25 ml.
5.6 Glass flasks with polytetrafluoroethylene (PTFE) lined screw caps with a capacity adapted to
the volume of the extract, e.g. 25 ml.
5.7 Disposable screw thread glass vials with a capacity of 1,5 ml and the corresponding
Polypropylene (PP) caps with silicone/PTFE gaskets.
6 Apparatus
6.1 Balance capable of accurately weighing 0,000 1 g.
6.2 Rotary evaporator.
6.3 Gas chromatograph coupled to a mass spectrometer (GC-MS).
5

---------------------- Page: 7 ----------------------
kSIST-TS FprCEN/TS 17630:2021
FprCEN/TS 17630:2021 (E)
7 Reagents
All reagents should be of analytical grade or better.
7.1 Water, grade 1 according to ISO 3696.
7.2 Ethanol, a volume fraction of 95 %.
7.3 Toluene, ≥ 99 %.
7.4 Acetone, ≥ 99 %.
7.5 Anthracene-d10 (internal standard), CAS N° 1719-06-8.
Commercial ready-to-use solutions at 10 mg/l in cyclohexene are available.
7.5.1 Intermediate solution of the internal standard at 800 µg/l in ethanol.
2 ml of the internal standard solution (7.5) are pipetted into a 25 ml volumetric flask and made up to
volume with ethanol (7.2).
7.6 Anthraquinone, C H O , CAS N° 84-65-1, ≥ 97%.
14 8 2
7.7 Solutions of anthraquinone
7.7.1 Stock solution of anthraquinone at 250 mg/l in toluene.
In a 100 ml volumetric flask, 25 mg ant
...

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