1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationAnalytical Method for theAnalysis of Propiconazole in treated Wood SamplesPD CEN/TR 16420:2012National forewordThis Published Document is the UK implementation of CEN/TR 16420:20
2、12. The UK participation in its preparation was entrusted to Technical CommitteeB/515, Wood preservation.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users ar
3、e responsible for its correct application. The British Standards Institution 2012.Published by BSI Standards Limited 2012.ISBN 978 0 580 78251 0 ICS 79.040Compliance with a British Standard cannot confer immunity from legal obligations.This Published Document was published under the authority of the
4、 Standards Policy and Strategy Committee on 31 December 2012.Amendments issued since publicationAmd. No. Date Text affectedPUBLISHED DOCUMENTPD CEN/TR 16420:2012TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN/TR 16420 October 2012 ICS 79.040 English Version Analytical Method for the Analy
5、sis of Propiconazole in treated Wood Samples Mthode danalyse du propiconazole dans des chantillons de bois trait Analyseverfahren zum Nachweis von Propiconazol in behandelten Holzproben This Technical Report was approved by CEN on 27 August 2012. It has been drawn up by the Technical Committee CEN/T
6、C 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,
7、Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any f
8、orm and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TR 16420:2012: EPD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Safety precautions .44 Principle 55 Reagents .56 Apparatus .57 Test sample 67.1 General 67.2 Dry matte
9、r content .68 Analytical procedure .68.1 General 68.2 Standard solutions 78.3 Determination .79 Calculation and expression of results .910 Quality assurance 911 Precision .912 Test report . 10Bibliography . 11PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 3 Foreword This document (CEN/TR 16420:2012) has
10、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 responsib
11、le for identifying any or all such patent rights. PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 4 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 (H
12、PLC). 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 li
13、mit lower than 1 g propiconazole/g and a quantification limit corresponding to 30 g propiconazole/g of wood material expressed as dry matter. It can be used over a measurement range up to a propiconazole content of 600 g/g of dry matter. NOTE 2 This method may need some modifications with some wood
14、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 do
15、cument (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
16、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
17、 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. PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 5 4 Principle Propiconazole is quantitatively extracted fr
18、om 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
19、CEN Technical Report should be demonstrated. Neither FID1)nor NPD2)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 interfer
20、e with the analytical results. 5.2 Methanol (CH3OH), 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 so
21、lvent or solvent mixture with that of methanol. 5.3 Propiconazole C15H17Cl2N3O2 CAS 60207-90-1 of certified purity: 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, su
22、pplied 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 m sieve. 6.2 Analytical balance, accurate to 0,1 mg. 6.3 Ultra-sonic bath equipped with a therm
23、ostat capable of controlling and maintaining a temperature of (50 1) C. 6.4 Adjustable volumetric micropipettes, 10 l, 100 l and 1000 l 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 inse
24、rt 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. PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 6 6.8 PTFE filte
25、rs 0,45 m 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 tw
26、o with a stationary phase of different polarity; length: 25 m to 30 m; internal diameter: 0,18 mm to 0,32 mm; film thickness: 0,25 m to 0,33 m. NOTE DB1, DB5, DB17 (phenyl)-methylpolysiloxane columns are examples of suitable products available commercially and supplied by Agilent J volume = 2 ml 6.1
27、3 High performance liquid chromatograph equipped with a UV detector or a diode array detector (DAD) for example. 6.14 HPLC column type C18 NOTE Analytical HPLC column type C18, particle size: 3 m to 5 m; length: 100 mm to 150 mm; internal diameter: 4,0 mm to 4,6 mm or similar. Suitable products avai
28、lable commercially: Purospher STAR RP 18 end capped; 5 m; 150 mm 4,6 mm, with pre-column C18, 4 mm 4 mm or Xterra MS C18; 3,5 m; 100 mm x 4,6 mm 6.15 A storage area (such as a refrigerator) capable of storing solutions at a temperature of no greater than 5 C. 7 Test sample 7.1 General Collect at lea
29、st 5 g of the sample material taken according to e.g. EN 212 or EN 351-2. Preferably under mild conditions without over heating, grind the sample material (e.g. cryogenic grinding) to particles with an approximate size lower than 1,0 mm diameter (passing through a 1000 m sieve). NOTE Wood shavings c
30、an also be prepared for analysis. However, it is recommended to cross check the extraction yield with that obtained when working on ground material. Homogenise the ground material to obtain a representative sample, and store it in a brown glass bottle with screw caps with a PTFE insert. This is the
31、test sample. 7.2 Dry matter content Approximately one half of the test sample is to be used to determine the moisture content of the sample. This is achieved by following the principles described in EN 13183-1. 8 Analytical procedure 8.1 General It is recommended to carry out at least two parallel a
32、nalyses. If the results differ by more than 10 %, an additional analysis shall be made. PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 7 8.2 Standard solutions 8.2.1 Preparation of stock solutions Weigh approximately 0,025 g of propiconazole to the nearest of 0,0001 g and transfer it quantitatively into
33、a 50 ml volumetric flask and make up to the mark with methanol. NOTE This stock solution with nominal concentrations of 500 mg/l can be stored at 5 C for at least twelve months. Avoid any temperature lower than 1 C. 8.2.2 Preparation of calibration standards To a series of five volumetric vials (6.6
34、) transfer respectively 0,3 ml, 1 ml, 2 ml, 5 ml and 10 ml of the stock solution (8.2.1). Make up to the mark with methanol. This gives a series of calibration standards with a propiconazole concentration of 3 g/ml, 10 g/ml, 20 g/ml, 50 g/ml and 100 g/ml respectively. NOTE Alternative method for cal
35、ibration standards preparation is to weigh all materials on a 4 decimal place balance rather than by volume. 5 calibration standards are prepared with approximate propiconazole concentration of 3 g/g, 10 g/g, 20 g/g, 50 g/g and 100 g/g. The maximum storage time of these solutions is two weeks at max
36、. 5 C, e.g. in a refrigerator. Avoid any temperature lower than 1 C. 8.3 Determination 8.3.1 Extraction Weigh, to the nearest 0,1 mg, approximately 1 g of the test sample (6.12) and transfer it to an extraction tube (6.7). With a pipette (6.5) add exactly 20,0 ml of methanol to the test sample, ensu
37、re that all the wood is wet. Close the tube with the screw cap. Place the tube in the ultra-sonic bath for 2 h at a temperature of 50 C. Shake it vigorously every 30 min. Allow the wood to settle and the solution to cool down. Filter the solution through a 0,45 m porosity filter (6.8) in order to av
38、oid column contamination by wood particles. Appropriate conditions should be applied in order to minimize solvent evaporation. Using a Pasteur pipette transfer 1 ml or 2 ml of the solution into a GC vial (6.6) or HPLC vial (6.12). Seal the vial with an appropriate cap. NOTE Other extraction techniqu
39、es, like Soxhlet extraction, microwave assisted extraction and pressurized fluid extraction (e.g. ASE) have been reported to be suitable. However, when using other extraction techniques the comparability to the method described in this CEN Technical Report should be demonstrated. 8.3.2 Gas chromatog
40、raphy (GC) 8.3.2.1 GC conditions Guidance on the gas chromatographic conditions is given in the following: Carrier gas: helium (minimum purity 99,9996 %); Gas flow: 20 cm/s to 30 cm/s; Make-up: argon-methane 95:5 Injection mode: preferably splitless/split, 1 l (any other non-discriminating injection
41、 technique is applicable); PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 8 Injector temperature: 250 C; Detector temperature: 350 C; Oven temperature programme: 90 C for 2 min; 45 C /min to 300 C hold for 5 min. Please consult the user instructions of the manufacturer for the optimal GC conditions. 8.3.
42、3 High Performance Liquid Chromatography (HPLC) 8.3.3.1 HPLC conditions Guidance on the HPLC conditions is given in the following: Temperature: 25 C Injection volume: 15,0 l Wavelength: 223 nmElution solvents: A acetonitrile B 0,5 % (m/v) ammonium carbonate solution Gradient: Time Flow A B (min) (ml
43、/min) 0 1,50 50 504 1,50 50 50 6 1,50 100 0 7 1,50 100 0 9 1,50 50 50 12 1,50 50 50Retention time: Propiconazole about 7,5 min (Purospher STAR column see NOTE 1) NOTE 1 If the expected content of the treated wood sample is higher than 1000 g propiconazole / g wood, the extract should be diluted befo
44、re the HPLC analysis in order to keep the propiconazole concentration within the calibration range (5 g/ml to 100 g/ml). NOTE 2 It may be necessary to change the wavelength or ratio of the elution solvents to avoid interfering wood extractives. 8.3.4 Calibration 8.3.4.1 General The linear calibratio
45、n function is based on five calibration points as described in (8.2.2). The calibration curve is established by plotting the ratio of the peak area of the propiconazole standard in function of the corresponding concentration. NOTE 1 The calibration can also be carried out using the internal standard
46、 method. PD CEN/TR 16420:2012CEN/TR 16420:2012 (E) 9 NOTE 2 A Quality Control (QC) procedure is added to validate calibration. The QC procedure can be a set of calibration solutions from another supplier. NOTE 3 For some column types avoid elution with 100 % organic solvent. 8.3.4.2 Validity check o
47、f the calibration curve The validity of the calibration curve shall be checked within each batch of samples by analysis of calibration solutions as unknown analytical samples (e.g. two for every ten samples). If the linear function calculated from these control measurements falls within the 95 % con
48、fidence interval of the actual calibration function, this function is assumed to be valid. If not, a new calibration function shall be established. 9 Calculation and expression of results The propiconazole concentration in the wood sample, in milligrams per kilogram of the test sample is calculated
49、from the multiple point linear calibration curve using the following relation: mVCC=extractpropicowhere Cpropicois the concentration of propiconazole, expressed in mg/kg dry wood; V is the extraction volume, expressed in ml (usually 20 ml); m is the sample dry mass, expressed in g (usually 1 g). Cextractis the concentration of propiconazole in g/ml in the extract given by the calibration curve or calculated f
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