EN ISO 15320:2003
(Main)Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO 15320:2003)
Pulp, paper and board - Determination of pentachlorophenol in an aqueous extract (ISO 15320:2003)
ISO 15320:2004 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.
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
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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.
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
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)
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 kilogram
of material.
4 Apparatus
4.1 Ordinary laboratory apparatus
4.2 Solid phase extraction (SPE) system and SPE columns
Propylphenyl columns, dimension 500 mg/3 ml.
4.3 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.
4.4 Capillary column
suitable for determination of acetylated derivates of pentachlorophenol. A column with the following features is
given as an example.
- stationary phase: polydimethylsiloxane with 5 % phenyl groups
- film thickness: 0,25 μm
- length: 30 m
- internal diameter: 0,32 mm.
4.5 Detector
electron capture detector (ECD)
or
mass spectrometer (MS) with the following features is given as an example:
a) ionisation: EI 70 eV (electron impact)
b) resolution: 1 amu (atomic mass unit)
c) runability: SIM mode (selected ion monitoring) (SIM is called SIR, selected ion recording for some
instruments)
5 Reagents
5.1 General
All reagents shall be of a grade “pro analysis” (p.a.) or equivalent quality, respectively water of grade 2 according to
EN ISO 3696:1995.
5.2 Methanol,
CH OH.
5.3 Hydrochloric acid,
HCl (0,1 mol/l).
5.4 n-Hexane,
C H .
6 14
5.5 Sulphuric acid,
H SO (diluted 1+1).
2 4
5.6 Acetic anhydride,
C H O (99 %).
4 6 3
5.7 Potassium carbonate solution,
K CO (0,1 mol/l). Weigh 13,8 g potassium carbonate with an accuracy of 0,1 g and dissolve it in a beaker with a
2 3
small amount of water. Transfer the solution to a 1000 ml volumetric flask and dilute to volume with water.
5.8 Reference solutions (for ECD)
5.8.1 Pentachlorophenol in methanol reference stock solution,
100 μg/ml. This solution is commercially available.
5.8.2 Pentachlorophenol in methanol dilute reference stock solution,
5 μg/ml. Pipette 1 ml of the stock solution (5.8.1) into a 20 ml volumetric flask and dilute to volume with methanol.
Solution is stable more than 6 months in the refrigerator.
5.8.3 Pentachlorophenol in methanol reference solution,
0,5 μg/ml. Pipette 1 ml of the dilute stock solution (5.8.2) into a 10 ml volumetric flask and dilute to volume with
methanol. Solution is stable more than 3 months in the refrigerator.
5.9 Internal standard solutions for ECD
5.9.1 2,3,6-trichlorophenol internal standard stock solution,
10 μg/ml, internal standard stock solution. This solution is commercially available.
5.9.2 2,3,6-trichlorophenol internal standard solution,
2 μg/ml, internal standard solution. Pipette 2 ml of the internal standard stock solution (5.9.1) into a 10 ml
volumetric flask and dilute to volume with methanol. Solution is stable more than 3 months in the refrigerator.
5.10 Internal standard solutions for MS
5.10.1 C6 labelled pentachlorophenol (labelled at all six carbons) internal standard stock solution,
10 μg/ml, internal standard stock solution. This solution is commercially available. It is an alternative to the 2, 3, 6-
trichlorophenol methanol solution mentioned in 5.9.1 and can be applied only when a mass spectrometer is used
...
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