CEN/TR 16420:2012

Analytical Method for the Analysis of Propiconazole in treated Wood Samples

This CEN Technical Report specifies a laboratory method for determining the content of propiconazole in treated wood using either Gas Chromatography (GC) or High Performance Liquid Chromatography (HPLC).
The method is aiming at determining the treatment quality at the time of treatment.
NOTE 1   Under appropriate circumstances the method is applicable for tebuconazole-treated wood as well as for the analysis of waste timber with respect to its propiconazole content.
The method has a detection limit lower than 1 µg propiconazole/g and a quantification limit corresponding to 30 µg propiconazole/g of wood material expressed as dry matter. It can be used over a measurement range up to a propiconazole content of 600 µg/g of dry matter.
NOTE 2   This method may need some modifications with some wood species such as hardwoods.

Analyseverfahren zum Nachweis von Propiconazol in behandelten Holzproben

Dieser Europäische Technische Bericht legt ein Laborverfahren zur Bestimmung des Gehalts an Propiconazol
in behandeltem Holz unter Anwendung entweder der Gaschromatographie (GC) oder der
Hochleistungsflüssigkeitschromatographie (HPLC) fest.
Das Verfahren zielt darauf ab, die Qualität der Behandlung zum Zeitpunkt dieser Behandlung zu bestimmen.
ANMERKUNG 1 Unter den geeigneten Umständen ist das Verfahren sowohl auf mit Tebuconazol behandeltes Holz als
auch für die Analyse von Altholz in Bezug auf dessen Propiconazol-Gehalt anwendbar.
Das Verfahren weist eine Nachweisgrenze von weniger als 1 µg Propiconazol/g und eine Bestimmungsgrenze
entsprechend 30 µg Propiconazol/g Holzmaterial auf, angegeben als Trockenmasse. Es kann über einen
Messbereich bis zu einem Propiconazolgehalt von 600 µg/g Trockenmasse angewendet werden.
ANMERKUNG 2 Dieses Verfahren erfordert bei einigen Holzarten, wie z. B. Laubhölzern, möglicherweise bestimmte
Veränderungen.

Méthode d'analyse du propiconazole dans des échantillons de bois traité

Le présent Rapport technique spécifie une méthode de détermination en laboratoire de la teneur en
propiconazole présent dans le bois traité, au moyen de la chromatographie en phase gazeuse (GC) ou de la
chromatographie liquide à haute performance (HPLC).
La méthode vise à déterminer la qualité du traitement au moment du traitement.
NOTE 1 La méthode est applicable, dans des conditions appropriées, tant au bois traité au tébuconazole qu’à l’analyse
du bois de rebut en ce qui concerne la teneur en propiconazole.
La limite de détection de la méthode est inférieure à 1 mg de propiconazole/g de bois et sa limite de
quantification correspond à 30 mg de propiconazole/g de bois exprimé en matière sèche. La méthode peut
être utilisée pour une teneur en propiconazole comprise dans une plage de mesures allant jusqu’à 600 mg de
propiconazole/g de matière sèche.
NOTE 2 La présente méthode peut nécessiter des modifications quand elle est utilisée sur des essences de bois
comme les bois de feuillus.

Analitska metoda za analizo propikonazola v obdelanih vzorcih lesa

To tehnično poročilo CEN določa laboratorijsko metodo za ugotavljanje vsebnosti propikonazola v obdelanem lesu s plinsko kromatografijo (GC) ali tekočinsko kromatografijo visoke ločljivosti (HPLC). Cilj metode je ugotoviti kakovost obdelave v času obdelave. Meja detekcije metode je nižja od 1 μg propikonazola na gram, meja kvantifikacije pa ustreza 30 μg propikonazola na gram lesnega materiala, izraženega s suho snovjo. Uporabi se lahko za merilno območje do 600 μg vsebnosti propikonazola na gram suhe snovi.

General Information

• Status: Published
• Publication Date: 23-Oct-2012
• ICS: 79.040 - Wood, sawlogs and sawn timber
• Technical Committee: CEN/TC 38 - Durability of wood and derived materials
• Drafting Committee: CEN/TC 38/WG 26 - Physical/chemical factors (analytical methods)
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 24-Oct-2012
• Due Date: 03-Oct-2013
• Completion Date: 24-Oct-2012
• Ref Project: SIST-TP CEN/TR 16420:2013 - Analytical Method for the Analysis of Propiconazole in Treated Wood Samples

Overview

CEN/TR 16420:2012 specifies a validated laboratory analytical method for measuring propiconazole in treated wood. The method uses solvent extraction (typically methanol) followed by instrumental analysis by Gas Chromatography (GC) or High Performance Liquid Chromatography (HPLC) to determine treatment quality at the time of application. Detection limit is < 1 µg propiconazole/g (dry wood) and the quantification limit is 30 µg/g; the method is validated up to about 600 µg/g dry matter.

Key topics and technical requirements

• Scope and purpose: Quantitative determination of propiconazole in treated timber; under certain conditions also applicable to tebuconazole or waste timber analysis. May require method adjustments for some hardwood species.
• Sampling & sample prep: Follow EN 212 / EN 351-2 guidance. Grind to pass a 1000 µm sieve (preferably <1.0 mm), homogenize and determine dry matter per EN 13183-1. Typical sample mass ~1 g for extraction; collect at least 5 g representative material.
• Extraction: Methanol extraction (20.0 ml per ~1 g sample) with ultrasonic bath at 50 ±1 °C for 2 hours, periodic agitation; filter through 0.45 µm PTFE filter. Alternative extraction techniques (Soxhlet, ASE, microwave) may be used if comparability is demonstrated.
• Instrumentation & detectors: GC with electron-capture detector (ECD) or GC–MS, and HPLC with UV or diode-array detector (DAD). Note: FID and some nitrogen-phosphorus detectors are generally not recommended based on interlaboratory validation.
• Calibration & quantification: Five-point linear calibration (nominal 3–100 µg/ml), stock solution ~500 mg/L. Calibration linearity r > 0.985; typical robust standard deviation from interlaboratory studies ~8–12%.
• Performance limits: Detection <1 µg/g; LOQ 30 µg/g; usable up to ~600 µg/g (dilution required if extracts exceed calibration range).

Applications and users

• Quality control at wood treatment plants to verify preservative uptake and treatment quality
• Testing laboratories performing regulatory compliance or product certification
• Manufacturers of wood preservatives and treated timber
• Waste timber characterization and recycling facilities (propiconazole content)
• Research institutions studying wood durability, preservative distribution, or extraction efficiency

Related standards

• EN 212 - Sampling and preparation for analysis of wood preservatives
• EN 351-2 - Guidance on sampling preservative-treated solid wood
• EN 13183-1 - Moisture/dry matter determination for sawn timber

Keywords: CEN/TR 16420, propiconazole analysis, treated wood, GC-ECD, HPLC-UV, wood preservatives, analytical method, extraction, detection limit, quantification limit.

Standards Content (Sample)

SLOVENSKI STANDARD
01-januar-2013
Analitska metoda za analizo propikonazola v obdelanih vzorcih lesa
Analytical Method for the Analysis of Propiconazole in Treated Wood Samples
Analyseverfahren zum Nachweis von Propiconazol in behandelten Holzproben
Méthode d'analyse du propiconazole dans des échantillons de bois traité
Ta slovenski standard je istoveten z: CEN/TR 16420:2012
ICS:
79.040 Les, hlodovina in žagan les Wood, sawlogs and sawn
timber
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 16420
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
October 2012
ICS 79.040
English Version
Analytical Method for the Analysis of Propiconazole in treated
Wood Samples
Méthode d'analyse du propiconazole dans des échantillons Analyseverfahren zum Nachweis von Propiconazol in
de bois traité behandelten Holzproben

This Technical Report was approved by CEN on 27 August 2012. It has been drawn up by the Technical Committee CEN/TC 38.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16420:2012: E
worldwide for CEN national Members.

Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Safety precautions .4
4 Principle .5
5 Reagents .5
6 Apparatus .5
7 Test sample .6
7.1 General .6
7.2 Dry matter content .6
8 Analytical procedure .6
8.1 General .6
8.2 Standard solutions .7
8.3 Determination .7
9 Calculation and expression of results .9
10 Quality assurance .9
11 Precision .9
12 Test report . 10
Bibliography . 11

Foreword
This document (CEN/TR 16420:2012) has been prepared by Technical Committee CEN/TC 38 “Durability of
wood and wood-based products”, the secretariat of which is held by AFNOR.
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.
1 Scope
This CEN Technical Report specifies a laboratory method for determining the content of propiconazole in
treated wood using either Gas Chromatography (GC) or High Performance Liquid Chromatography (HPLC).
The method is aiming at determining the treatment quality at the time of treatment.
NOTE 1 Under appropriate circumstances the method is applicable for tebuconazole-treated wood as well as for the
analysis of waste timber with respect to its propiconazole content.
The method has a detection limit lower than 1 µg propiconazole/g and a quantification limit corresponding to
30 µg propiconazole/g of wood material expressed as dry matter. It can be used over a measurement range
up to a propiconazole content of 600 µg/g of dry matter.
NOTE 2 This method may need some modifications with some wood species such as hardwoods.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
EN 212, Wood preservatives – General guidance on sampling and preparation for analysis of wood
preservatives and treated timber
EN 351-2, Durability of wood and wood-based products – Preservative treated solid wood – Part 2: Guidance
on sampling for the analysis of preservative-treated wood
EN 13183-1, Moisture content of a piece of sawn timber – Part 1: Determination by oven dry 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 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
Propiconazole is quantitatively extracted from the wood material using methanol. The extracted compounds
are analysed by GC-ECD, GC-MS, GC-NPD, HPLC-UV or HPLC-DAD.
NOTE Other analytical techniques have been reported to be adequately applicable. However, when using other
analytical techniques the comparability to the method described in this CEN Technical Report should be demonstrated.
1) 2)
Neither FID nor NPD detectors are expected to be appropriate detecting devices.
5 Reagents
5.1 General
During the analysis, unless otherwise specified, use only reagents of recognised analytical grade that have
been checked in advance as to not interfere with the analytical results.
5.2 Methanol (CH OH), analytical grade.
NOTE Other solvents may be used instead of methanol (e.g. ethylacetate) as some extraction difficulties may 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 Propiconazole [C H Cl N O ] [CAS 60207-90-1] of certified purity:
15 17 2 3 2
 purity >98 % - mixture of stereo isomers (e.g. Pestanal from Sigma-Aldrich, cat. 45642),
 alternatively, (typical purity 50 %) - mixture of stereo isomers, from Janssen Pharmaceutica, supplied
with Certificate of Analysis.
6 Apparatus
Ordinary laboratory apparatus and the following:
6.1 Grinder, capable of grinding timber samples such that the resultant particles will pass through a 1000
µm sieve.
6.2 Analytical balance, accurate to 0,1 mg.
6.3 Ultra-sonic bath equipped with a thermostat capable of controlling and maintaining a temperature of
(50 ± 1) °C.
6.4 Adjustable volumetric micropipettes, 10 µl, 100 µl and 1000 µl full capacity.
6.5 Volumetric pipettes, 10 ml capacity.
6.6 Volumetric flasks, 50 ml capacity.
6.7 Glass tubes 30 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.
1) Concluded from the 2007 round robin test.
2) Concluded from the 2008 round robin test.
6.8 PTFE filters 0,45 µm porosity with supporting device.
6.9 2 ml GC vials with sealed caps.
6.10 Gas chromatograph equipped with a splitless/split or a non-discriminating injection system and an
electron capture detector (ECD) for example.
6.11 Semi-polar separation column. One capillary column, or preferably two with a stationary phase of
different polarity; leng
...