Durability of wood and wood-based products - Quantitative determination of pentachlorophenol in wood - Gas chromatographic method

This Technical Report specifies a laboratory method of determining the pentachlorophenol content of wood. The method is applicable to all types of PCP- treated wood and wood-based materials as well as for the analysis of waste timber with respect to its PCP content.
The method has a quantification limit corresponding to 100 µg PCP per kilogram of wood material expressed as dry matter. The method described has a measurement range up to PCP contents of 25 mg/kg of dry matter. These figures refer to the given example (where an aliquot of 1 ml of the extract is used for acetylation, see 8.4).
NOTE 1   If lower quantification limits are required, a higher volume of extract aliquot can be used for derivatisation.
NOTE 2    This method could have some modifications with some wood species as hardwoods.

Dauerhaftigkeit von Holz und Holzprodukten - Quantitative Bestimmung von Pentachlorphenol in Holz - Gaschromatographische Verfahren

Dieser Europäische Technische Bericht beschreibt ein Laborverfahren zur Bestimmung des Pentachlorphenol-Gehalts von Holz. Das Verfahren kann bei behandeltem Holz und Holzwerkstoffen angewendet werden.
Die Bestimmungsgrenze des Verfahrens liegt bei 100 mg PCP/kg Holz, bezogen auf die Trockensubstanz. Das beschriebene Verfahren ist anwendbar bis zu einem PCP-Gehalt von 25 mg/kg Trockensubstanz. Diese Angaben beziehen sich auf das angegebene Beispiel (in dem ein Aliquot von 1 ml des Extraktes für die Acetylierung verwendet wird, siehe 8.4).
ANMERKUNG 1   Sind niedrigere Bestimmungsgrenzen erforderlich, kann ein größeres Extraktvolumen als Aliquot für die Derivatisierung verwendet werden.
ANMERKUNG 2   Bei einigen Holzarten, wie z. B.Laubholz, können Änderungen dieses Verfahrens erforderlich sein.

Durabilité du bois et des matériaux dérivés du bois - Analyse quantitative du pentachlorophénol dans le bois - Méthode par chromatographie en phase gazeuse

Ce Rapport Technique décrit une méthode de laboratoire de détermination de la teneur en pentachlorophénol du bois. La méthode s'applique à tous types de bois ou matériau à base de bois traité avec du PCP ainsi qu'à l'analyse de déchets de bois quant à leur teneur en PCP.
La limite de quantification de la méthode correspond à 100 mg de PCP/kg de bois exprimé en matière sèche. La gamme de mesure dans la méthode décrite va jusqu'à une teneur de 25 mg/kg de matière sèche. Ces chiffres se réfèrent à l'exemple donné (dans lequel un aliquote de 1ml de l'extrait est utilisé pour l'acétylation, voir 8.4).
NOTE 1   Si des limites de quantification inférieures ont exigées, il est possible d'utiliser un extrait aliquote de plus grand volume.
NOTE 2   Il est possible d'apporter quelques modifications à cette méthode pour quelques essences de bois telles que des feuillus

Trajnost lesa in lesnih proizvodov – Kvantitativno določanje pentaklorofenola v lesu – Plinska kromatografska metoda

General Information

Status
Published
Publication Date
16-Sep-2003
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
17-Sep-2003
Completion Date
17-Sep-2003

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SLOVENSKI STANDARD
SIST-TR CEN/TR 14823:2004
01-januar-2004
7UDMQRVWOHVDLQOHVQLKSURL]YRGRY±.YDQWLWDWLYQRGRORþDQMHSHQWDNORURIHQRODY
OHVX±3OLQVNDNURPDWRJUDIVNDPHWRGD
Durability of wood and wood-based products - Quantitative determination of
pentachlorophenol in wood - Gas chromatographic method
Dauerhaftigkeit von Holz und Holzprodukten - Quantitative Bestimmung von
Pentachlorphenol in Holz - Gaschromatographische Verfahren
Durabilité du bois et des matériaux dérivés du bois - Analyse quantitative du
pentachlorophénol dans le bois - Méthode par chromatographie en phase gazeuse
Ta slovenski standard je istoveten z: CEN/TR 14823:2003
ICS:
79.040 Les, hlodovina in žagan les Wood, sawlogs and sawn
timber
SIST-TR CEN/TR 14823:2004 en

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

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SIST-TR CEN/TR 14823:2004
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SIST-TR CEN/TR 14823:2004
TECHNICAL REPORT
CEN/TR 14823
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
September 2003
ICS 71.100.50; 79.040
English version
Durability of wood and wood-based products – Quantitative
determination of pentachlorophenol in wood – Gas
chromatographic method

Durabilité du bois et des matériaux dérivés du bois – Dauerhaftigkeit von Holz und Holzprodukten – Quantitative

Analyse quantitative du pentachlorophénol dans le bois – Bestimmung von Pentachlorphenol in Holz –

Méthode par chromatographie en phase gazeuse Gaschromatographische Verfahren

This Technical Report was approved by CEN on 27 July 2003. It has been drawn up by the Technical Committee CEN/TC 38.

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. CEN/TR 14823:2003 E

worldwide for CEN national Members.
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SIST-TR CEN/TR 14823:2004
CEN/TR 14823:2003 (E)
Contents
Page

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

Introduction .................................................................................................................................................................4

1 Scope ..............................................................................................................................................................5

2 References......................................................................................................................................................5

3 Safety precautions.........................................................................................................................................5

4 Principle..........................................................................................................................................................5

5 Reagents.........................................................................................................................................................5

6 Apparatus .......................................................................................................................................................6

7 Preparation of the test sample .....................................................................................................................7

8 Procedure .......................................................................................................................................................7

8.1 General...................................................................................................................................................................7

8.2 Standard solutions ...............................................................................................................................................7

8.3 Preparation of the calibration solutions.............................................................................................................8

8.4 Determination........................................................................................................................................................8

9 Calculation and expression of results.......................................................................................................10

10 Quality assurance ........................................................................................................................................11

11 Precision.......................................................................................................................................................11

12 Test report ....................................................................................................................................................11

Annex A Ring test results ........................................................................................................................................12

Bibliography ..............................................................................................................................................................13

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SIST-TR CEN/TR 14823:2004
CEN/TR 14823:2003 (E)
Foreword

This document (CEN/TR 14823:2003) has been prepared by Technical Committee CEN/TC 38 “Durability of wood

and wood-based products”, the secretariat of which is held by AFNOR.

This status of this document as Technical Report has been chosen because this method described is an example

of a laboratory method validated by a ring test. It is recognized that, for example, different techniques of extraction

might be employed by the analyst without loss of analytical performance and quality. However, when using different

techniques the comparability to the method described in this Technical Report should be demonstrated, e.g. by

using a certified reference material (CRM).
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SIST-TR CEN/TR 14823:2004
CEN/TR 14823:2003 (E)
Introduction

At present, no standardised method for the analysis of pentachlorophenol (PCP) in wood is recognized in Europe.

Only a few national standards are available world wide, e g BS 5666, Part 6 and AWPA Standard A-5 and these

methods are designed for the analysis of timber treated with levels of PCP that are necessary to prevent

degradation of the treated timber by fungi.

This Technical Report has been issued in order to facilitate the analysis of PCP-treated wood and panels and in

particular low levels of PCP that can be present in packaging timbers and pallets. Low levels of PCP and other

chlorophenols, and the anisoles derived from them, can cause taints in foodstuffs. PCP can be present as residues

from old anti-sapstain treatment or some timber treated against decay could inadvertently have been incorporated

into the panel product.
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CEN/TR 14823:2003 (E)
1 Scope

This Technical Report specifies a laboratory method of determining the pentachlorophenol content of wood. The

method is applicable to all types of PCP- treated wood and wood-based materials as well as for the analysis of

waste timber with respect to its PCP content.

The method has a quantification limit corresponding to 100 μg PCP per kilogram of wood material expressed as dry

matter. The method described has a measurement range up to PCP contents of 25 mg/kg of dry matter. These

figures refer to the given example (where an aliquot of 1 ml of the extract is used for acetylation, see 8.4).

NOTE 1 If lower quantification limits are required, a higher volume of extract aliquot can be used for derivatisation.

NOTE 2 This method could have some modifications with some wood species as hardwoods.

2 References

EN 212, Wood preservatives - General guidance on sampling and preparation for analysis of wood preservatives

and treated timber.
EN 322, Wood-based panels – Determination of moisture content.

EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).

ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the

determination of repeatability and reproducibility of a standard measurement method.

ISO 11465, Soil quality - Determination of dry matter and water content on a mass basis - Gravimetric method.

3 Safety precautions

Persons using this method should be familiar with normal analytical laboratory procedures and practice.

This method does not purport to address all the safety problems, if any, associated with its use.

It is the responsibility of the user to establish safety and health practices and to ensure compliance with any

European or national regulatory conditions.
4 Principle

Pentachlorophenol is extracted from the wood material using methanol. The extracted pentachlorophenol is

transformed to pentachlorophenol acetate by derivatisation of an aliquot of the extract in aqueous potassium

carbonate solution with acetic anhydride. The acetate derivative formed is extracted from this aqueous solution with

n-hexane and analysed by gas chromatography with electron capture detection.
5 Reagents

During the analysis, unless otherwise specified, use only reagents of recognized analytical grade which have been

checked in advance as to not interfere with the analytical results, and water complying with grade 3 as defined in

EN ISO 3696.
5.1 Acetic anhydride (C H O ).
4 6 3
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5.2 Methanol (CH OH).

NOTE Other solvents can be used instead of methanol, some extraction difficulties can occur with some wood species

(e.g. hardwoods). It is recommended to cross check the extraction efficiency of any other solvent or solvent mixture with that of

methanol.
5.3 n-Hexane (C H ).
6 14
5.4 Potassium carbonate, solution, c(K CO ) = 0,1 mol/l.
5.5 Sodium sulfate, anhydrous (Na SO ).
2 4

5.6 Pentachlorophenol (PCP, (C Cl OH)) of certified purity (> 99%), e.g. IPO 560 .

6 5

5.7 2,4,6-tribromophenol (TBP, (C H Br OH)) of certified purity (> 98%) as an internal standard.

6 2 3
5.8 Purified sand, (ignited at 900 °C after acid treatment)

NOTE An untreated wood sample (of the same wood species as the sample for analysis) known to be free of

pentachlorophenol can also be used instead of purified sand but before use it should be checked for interference with the

analytical method.
6 Apparatus
Ordinary laboratory apparatus and the following.
NOTE Glassware should be thoroughly cleaned prior to use.
6.1 Analytical balance, accurate to 0,01 mg.

6.2 Ultra-sonic bath equipped with a thermostat capable of controlling and maintaining a temperature of 40 °C.

6.3 Disposable Pasteur pipettes made of glass, 2,0 ml capacity.
6.4 Separating funnel, 150 ml capacity.
6.5 Volumetric pipettes, 1,0 ml and 10 ml or 20 ml capacity.
6.6 Microlitre syringes, 25 μl, 100 μl and 500 μl capacity.
6.7 Volumetric flasks, 10 ml, 25 ml and 50 ml capacity.

6.8 Conical flasks 100 ml capacity, with screw caps provided with an insert of polytetrafluoroethylene (PTFE) or

alternatively with standard ground stoppers provided with PTFE standard ground sockets and conical joint clips.

6.9 Gas chromatograph equipped with a splitless/split or a non-discriminating injection system and an electron

capture detector (ECD)

6.10 Separation column. One capillary column, or preferably two, with stationary phase of different polarity e.g.

DB 1, DB 5, DB 17 ; length: 25 m to 30 m; internal diameter: 0,2 mm to 0,32 mm; film thickness: 0,25 μm to 0,33

μm.

1) IPO 560 is an example of a suitable product available commercially, supplied by Promochem. This information is given for

the convenience of users of this CEN Technical Report and does not constitute and endorsement by CEN of this product.

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CEN/TR 14823:2003 (E)
6.11 Pre-column coated with deactivated silica.
7 Preparation of the test sample

Collect at least 10 g of the sample material taken according to e.g. EN 212. This sample material is preferably

ground under mild conditions (e.g. cryogenic grinding) to chips with an approximate particle size of 0,5 mm to 1,0

mm diameter.

NOTE 1 Wood shavings can also be made for analysis (especially if other compounds e.g. trichlorophenols or

trichloroanisols have to be analysed at the same time).

Homogenise the ground sample material to obtain a representative sample, and store it in a brown glass vessel

with screw caps with a PTFE insert. This is the test sample.

NOTE 2 If possible, the sample for analysis should be prepared from a minimum of five independent pieces or sections

representatively taken from the quantity of wood material to be analysed.
8 Procedure
8.1 General

It is recommended to carry out at least two parallel analyses. If results differ by more than 10 % an additional

analysis shall be carried out.
8.2 Standard solutions
8.2.1 Preparation of stock solutions (calibrant and internal standard)

Prepare the stock solutions by weighing about 12,5 mg of PCP (5.6) and TBP (5.7) separately to the nearest of

0,01 mg and dissolve each in 25 ml methanol (5.2).

NOTE These stock solutions with nominal concentrations of 0,5 mg/ml can be stored in the dark at –18 °C for three

months.
8.2.2 Preparation of working solutions

Transfer by pipette (6.5) 1,00 ml of stock PCP solution (8.2.1) to a 10 ml one-mark volumetric flask and make up to

the mark with methanol (5.2) to give
...

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