Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO 15320:2003)

This European Standard specifies a test method for the determination of the total content of pentachlorophenol (PCP) in pulp, paper and board. Though it is developed for paper and board intended to come into contact with foodstuffs, it is applicable to all kinds of pulp, paper and board. The limit of determination is 0,05 micrograms per gram of pulp, paper and board.

Halbstoff, Papier und Pappe - Bestimmung von Pentachlorphenol in einem wässrigen Extrakt (ISO 15320:2003)

Pâtes, papier et carton - Détermination du pentachlorophénol dans un extrait aqueux (ISO 15320:2003)

L'ISO 15320:2004 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.

Papir, karton in lepenka – Določevanje pentaklorofenola v vodnem ekstraktu (ISO 15320:2003)

General Information

Status
Withdrawn
Publication Date
31-Jan-2004
Withdrawal Date
09-Oct-2011
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
05-Oct-2011
Due Date
28-Oct-2011
Completion Date
10-Oct-2011

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Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 15320:2004
01-februar-2004
3DSLUNDUWRQLQOHSHQND±'RORþHYDQMHSHQWDNORURIHQRODYYRGQHPHNVWUDNWX ,62


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

15320:2003)
Halbstoff, Papier und Pappe - Bestimmung von Pentachlorphenol in einem wässrigen
Extrakt (ISO 15320:2003)

Pâtes, papier et carton - Détermination du pentachlorophénol dans un extrait aqueux

(ISO 15320:2003)
Ta slovenski standard je istoveten z: EN ISO 15320:2003
ICS:
85.040 Vlaknine Pulps
85.060 Papir, karton in lepenka Paper and board
SIST EN ISO 15320:2004 en

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

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SIST EN ISO 15320:2004
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SIST EN ISO 15320:2004
EUROPEAN STANDARD
EN ISO 15320
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2003
ICS 85.040; 85.060
English version
Pulp, paper and board - Determination of pentachlorophenol in
an aqueous extract (ISO 15320:2003)

Pâtes, papier et carton - Détermination du Halbstoff, Papier und Pappe - Bestimmung von

pentachlorophénol dans un extrait aqueux (ISO Pentachlorphenol in einem wässrigen Extrakt (ISO

15320:2003) 15320:2003)
This European Standard was approved by CEN on 20 February 2003.

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 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 Management Centre has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,

Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United

Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15320:2003 E

worldwide for CEN national Members.
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SIST EN ISO 15320:2004
EN ISO 15320:2003 (E)
Content
Page

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

1 Scope ..............................................................................................................................................................3

2 Normative References ...................................................................................................................................3

3 Principle..........................................................................................................................................................4

4 Apparatus .......................................................................................................................................................4

4.1 Ordinary laboratory apparatus .....................................................................................................................4

4.2 Solid phase extraction (SPE) system and SPE columns...........................................................................4

4.3 Gas chromatograph.......................................................................................................................................4

4.4 Capillary column, ...........................................................................................................................................4

4.5 Detector...........................................................................................................................................................4

5 Reagents.........................................................................................................................................................4

5.1 General............................................................................................................................................................4

5.2 Methanol, ........................................................................................................................................................5

5.3 Hydrochloric acid,..........................................................................................................................................5

5.4 n-Hexane,........................................................................................................................................................5

5.5 Sulphuric acid, ...............................................................................................................................................5

5.6 Acetic anhydride, ...........................................................................................................................................5

5.7 Potassium carbonate solution,.....................................................................................................................5

5.8 Reference solutions (for ECD)......................................................................................................................5

5.9 Internal standard solutions for ECD ............................................................................................................5

5.10 Internal standard solutions for MS ..............................................................................................................6

6 Sampling and extraction ...............................................................................................................................6

7 Procedure .......................................................................................................................................................6

7.1 Preparation .....................................................................................................................................................6

7.2 Solid phase concentration............................................................................................................................6

7.3 Acetylation......................................................................................................................................................7

7.4 Gas chromatographic analysis.....................................................................................................................7

8 Calibration ......................................................................................................................................................7

8.1 Calibration for electron capture detector, ECD ..........................................................................................7

8.2 Calibration for mass spectrometer using 13C-labelled PCP.....................................................................8

9 Calculation......................................................................................................................................................8

10 Precision.........................................................................................................................................................9

11 Test report ......................................................................................................................................................9

Bibliography ..............................................................................................................................................................10

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SIST EN ISO 15320:2004
EN ISO 15320:2003 (E)
Foreword

This document (EN ISO 15320:2003) has been prepared by Technical Committee CEN/TC 172 "Pulp, paper and

board", the secretariat of which is held by DIN, in collaboration with Technical Committee ISO/TC 6 "Paper, board

and pulps".

This European Standard EN ISO 15320:2003 including the Amendment shall be given the status of a national

standard, either by publication of an identical text or by endorsement, at the latest by June 2004, and

conflicting national standards shall be withdrawn at the latest by June 2004.

WARNING: The use of this European Standard may involves hazardous materials, e.g. methanol and

pentachlorophenol, which are toxic substances, as well as acetic anhydryde, which is corrosive. This

European Standard does not address all the safety and environmental problems associated with its use. It

is the responsibility of the user of this European Standard to establish appropriate safety, health and

environmental practices and determine applicability of safety regulations prior to use.

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

countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,

Slovakia, Spain, Sweden, Switzerland and the United Kingdom.
1 Scope

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

extract in pulp, paper and board. Though it is developed for paper and board intended to come into contact with

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

NOTE 1 It was investigated that a hot water extract (acc. to EN 647) is sufficient for the determination of PCP in pulp, paper

and board.
The working range for the method is 0,05 mg/kg to 0,5 mg/kg.

NOTE 2 The upper limit of the working range could be increased if the aqueous extract is diluted.

2 Normative References

This European Standard incorporates by dated or undated reference, provisions from other publications. These

normative references are cited at the appropriate places in the text and the publications are listed hereafter. For

dated references, subsequent amendments to or revisions of any of these publications apply in this European

Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the

publication referred to applies (including amendments).

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 ISO 3696:1995 Water for analytical laboratory use – Specification and test methods (ISO 3696:1987)

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SIST EN ISO 15320:2004
EN ISO 15320:2003 (E)
3 Principle

A specimen of the material to be tested is extracted with cold water according to EN 645 or with hot water

according to EN 647. The pentachlorophenol in the extract is concentrated using solid phase extraction on a phenyl

column. The pentachlorophenol is then eluted from the phenyl column with hexane, acetylated using acetic

anhydride and the amount of pentachlorophenol present determined using gas chromatography employing an ECD

(electron capture detector) or MS (mass spectrometer) detector. The result is expressed as milligrams per kil

...

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