Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO 15320:2011)

This International Standard specifies a test method for the determination of pentachlorophenol (PCP) in an aqueous extract of pulp, paper and board. Although it was developed for paper and board intended to come into contact with foodstuffs, it is applicable to all kinds of pulp, paper and board. The working range for acetylation is 0,05 mg/kg to 0,5 mg/kg.

Zellstoff, Papier und Pappe - Bestimmung von Pentachlorphenol in einem wässrigen Extrakt (ISO 15320:2011)

Diese Internationale Norm legt ein Prüfverfahren zur Bestimmung von Pentachlorphenol (PCP) in einem
wässrigen Extrakt in Zellstoff, Papier und Pappe fest. Obwohl sie für Papier und Pappe, die mit Lebensmitteln
in Kontakt kommen, entwickelt wurde, ist sie auch für alle anderen Arten von Zellstoff, Papier und Pappe
anwendbar.
ANMERKUNG 1 Für die Bestimmung von PCP in Zellstoff, Papier und Pappe wurde festgestellt, dass ein
Heißwasserextrakt nach EN 647 zu zufriedenstellenden Ergebnissen führt.
Der Arbeitsbereich des Prüfverfahrens für beide Verfahren, Acetylierung und Silylierung, liegt zwischen
0,005 mg/kg bis 0,05 mg/kg.
ANMERKUNG 2 Falls der Wasserextrakt verdünnt ist, könnte sich der obere Grenzwert des Arbeitsbereiches erhöhen.
WARNHINWEIS — Die Anwendung dieser Internationalen Norm beinhaltet gefährliche Materialien, z.
B. die giftigen Substanzen Methanol und Pentachlorphenol sowie das ätzende Essigsäureanhydrid.
Diese Internationale Norm geht nicht auf alle Sicherheits- und Umweltprobleme ein, die mit ihrer
Anwendung verbunden sind. Der Anwender der Internationalen Norm ist dafür verantwortlich, dass
vor deren Benutzung geeignete Sicherheits-, umweltschützende und Gesundheitsmaßnahmen
getroffen sowie die Anwendung von Sicherheitsregeln festgelegt werden.

Pâtes, papiers et cartons - Dosage du pentachlorophénol dans un extrait aqueux (ISO 15320:2011)

L'ISO 15320:2011 spécifie une méthode d'essai pour le dosage du pentachlorophénol (PCP) dans un extrait aqueux de pâtes, papiers et cartons. Bien que développée pour les papiers et cartons destinés à entrer en contact avec les denrées alimentaires, elle est applicable à tous les types de pâtes, papiers et cartons.
La plage de travail pour l'acétylation est comprise entre 0,05 mg/kg et 0,5 mg/kg.

Lepenka, papir in karton - Določevanje pentaklorofenola v vodnem ekstraktu (ISO 15320:2011)

Ta mednarodni standard določa preskusno metodo za določevanje pentaklorofenola (PCP) v vodnem ekstraktu lepenke, papirja in kartona. Čeprav je bil razvit za papir in karton, ki je namenjen neposrednemu stiku z živili, velja za vse vrste lepenke, papirja in kartona. Delovni razpon za acetilacijo je med 0,05 mg/kg in 0,5 mg/kg.

General Information

Status
Published
Publication Date
12-Oct-2011
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
14-Sep-2011
Due Date
19-Nov-2011
Completion Date
13-Oct-2011

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SLOVENSKI STANDARD
SIST EN ISO 15320:2011
01-november-2011
1DGRPHãþD
SIST EN ISO 15320:2004
/HSHQNDSDSLULQNDUWRQ'RORþHYDQMHSHQWDNORURIHQRODYYRGQHPHNVWUDNWX ,62


Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO

15320:2011)
Zellstoff, Papier und Pappe - Bestimmung von Pentachlorphenol in einem wässrigen
Extrakt (ISO 15320:2011)

Pâtes, papiers et cartons - Dosage du pentachlorophénol dans un extrait aqueux (ISO

15320:2011)
Ta slovenski standard je istoveten z: EN ISO 15320:2011
ICS:
85.040 Vlaknine Pulps
85.060 Papir, karton in lepenka Paper and board
SIST EN ISO 15320:2011 en

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

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SIST EN ISO 15320:2011
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SIST EN ISO 15320:2011
EUROPEAN STANDARD
EN ISO 15320
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2011
ICS 85.040; 85.060 Supersedes EN ISO 15320:2003
English Version
Pulp, paper and board - Determination of pentachlorophenol in
an aqueous extract (ISO 15320:2011)

Pâtes, papiers et cartons - Dosage du pentachlorophénol Zellstoff, Papier und Pappe - Bestimmung von

dans un extrait aqueux (ISO 15320:2011) Pentachlorphenol in einem wässrigen Extrakt (ISO

15320:2011)
This European Standard was approved by CEN on 14 August 2011.

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. Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15320:2011: E

worldwide for CEN national Members.
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SIST EN ISO 15320:2011
EN ISO 15320:2011 (E)
Contents Page

Foreword ..............................................................................................................................................................3

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SIST EN ISO 15320:2011
EN ISO 15320:2011 (E)
Foreword

This document (EN ISO 15320:2011) has been prepared by Technical Committee ISO/TC 6 "Paper, board

and pulps" in collaboration with Technical Committee CEN/TC 172 “Pulp, paper and board” the secretariat of

which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of an identical

text or by endorsement, at the latest by February 2012, and conflicting national standards shall be withdrawn

at the latest by February 2012.

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.

This document supersedes EN ISO 15320:2003.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following

countries are bound to implement this European Standard: 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 and the United Kingdom.
Endorsement notice

The text of ISO 15320:2011 has been approved by CEN as a EN ISO 15320:2011 without any modification.

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SIST EN ISO 15320:2011
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SIST EN ISO 15320:2011
INTERNATIONAL ISO
STANDARD 15320
Second edition
2011-08-15
Pulp, paper and board — Determination
of pentachlorophenol in an aqueous
extract
Pâtes, papiers et cartons — Dosage du pentachlorophénol dans un
extrait aqueux
Reference number
ISO 15320:2011(E)
ISO 2011
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SIST EN ISO 15320:2011
ISO 15320:2011(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2011

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2011 – All rights reserved
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SIST EN ISO 15320:2011
ISO 15320:2011(E)
Contents Page

Foreword ............................................................................................................................................................ iv

1  Scope ...................................................................................................................................................... 1

2  Normative references ............................................................................................................................ 1

3  Principle ................................................................................................................................................. 1

4  Apparatus ............................................................................................................................................... 2

5  Reagents ................................................................................................................................................ 2

6  Sampling ................................................................................................................................................ 3

7  Extraction ............................................................................................................................................... 3

7.1  Cold-water extraction ............................................................................................................................ 3

7.2  Hot-water extraction .............................................................................................................................. 4

8  Procedure ............................................................................................................................................... 4

8.1  Preparation ............................................................................................................................................. 4

8.2  Solid phase concentration ................................................................................................................... 4

8.3  Derivatization ......................................................................................................................................... 4

9  Calibration .............................................................................................................................................. 5

10  Gas chromatographic analysis ............................................................................................................ 5

10.1  Gas chromatographic condition .......................................................................................................... 5

10.2  Establishing retention time of pentachlorophenol ............................................................................ 5

10.3  Calculation of the area ratio versus mass ratio ................................................................................. 5

10.4  Calibration for mass spectrometer using C labelled pentachlorophenol ................................. 6

11  Calculation ............................................................................................................................................. 6

12  Test report .............................................................................................................................................. 7

Annex A (informative) Precision ........................................................................................................................ 8

Bibliography ........................................................................................................................................................ 9

© ISO 2011 – All rights reserved iii
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SIST EN ISO 15320:2011
ISO 15320:2011(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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.

ISO 15320 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.

This second edition cancels and replaces the first edition (ISO 15320:2003), which has been technically

revised.
iv © ISO 2011 – All rights reserved
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SIST EN ISO 15320:2011
INTERNATIONAL STANDARD ISO 15320:2011(E)
Pulp, paper and board — Determination of pentachlorophenol
in an aqueous extract

WARNING — The use of this International Standard may involve hazardous materials, e.g. methanol

and pentachlorophenol, which are toxic substances, as well as acetic anhydride, which is corrosive.

This International Standard does not address all the safety and environmental problems associated

with its use. It is the responsibility of the user of this International Standard to establish appropriate

safety, health and environmental practices and determine the applicability of safety regulations prior

to use.
1 Scope

This International Standard specifies a test method for the determination of pentachlorophenol (PCP) in an

aqueous extract of pulp, paper and board. Although it was developed for paper and board intended to come

into contact with foodstuffs, it is applicable to all kinds of pulp, paper and board.

The working range for acetylation is 0,05 mg/kg to 0,5 mg/kg.

NOTE The upper limit of the working range could be increased if the aqueous extract is diluted.

2 Normative references

The following referenced documents are indispensable for the application 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.
ISO 186, Paper and board — Sampling to determine average quality
ISO 536, Paper and board — Determination of grammage

ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method

ISO 7213, Pulps — Sampling for testing
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Principle

A specimen of the material to be tested is extracted with either cold or hot water. The pentachlorophenol

extract is concentrated by adsorption onto a phenyl silica column using solid-phase extraction. The

pentachlorophenol is then eluted from the phenyl silica column with n-hexane and an acetylated derivative

formed with acetic anhydride. The amount of pentachlorophenol present is then determined using gas

chromatography employing an electron-capture detector (ECD) or mass spectrometer (MS) detector. The

result is expressed as milligrams per kilogram of material.
© ISO 2011 – All rights reserved 1
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SIST EN ISO 15320:2011
ISO 15320:2011(E)
4 Apparatus

4.1 Conical flask, 500 ml, wide necked with a ground-glass stopper with tap (see ISO 1773).

4.2 Filtration equipment, fritted-glass filter of porosity 4 (nominal size 90 μm) with a filter flask of 500 ml

(see ISO 6556).
4.3 Marked volumetric flask, 250 ml (see ISO 1042).

4.4 Solid-phase extraction (SPE) system and SPE columns, phenyl silica columns, 500 mg/3 ml.

4.5 Gas chromatograph, a conventional split/splitless injector gives suitable sensitivity when used in the

splitless mode. Alternatively, an on-column injection mode may be used.

4.6 Capillary column, suitable for determination of acetylated derivates of pentachlorophenol. A column

with the following features is given as an example:
 stationary phase: polydimethyl-siloxan with 5 % phenyl groups;
 film thickness: 0,25 µm;
 length: 30 m;
 internal diameter: 0,32 mm.

4.7 Detector, electron-capture detector (ECD) or mass spectrometer (MS) suitable for carrying out the

measurement. The following features are given as an example:
a) ionization: EI 70 eV (electron impact);
b) resolution: 1 amu (atomic mass
...

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