EN 1014-4-2010 en Wood preservatives - Creosote and creosoted timber - Methods of sampling and analysis - Part 4 Determination of the water-extractable phenols content of creosote《.pdf

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1、BS EN1014-4:2010ICS 71.100.50NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDWood preservatives Creosote and creosotedtimber Methods ofsampling and analysisPart 4: Determination of the water-extractable phenols content of creosoteThis British Standardwas publish

2、ed under theauthority of the StandardsPolicy and StrategyCommittee on 31 July 2010 BSI 2010ISBN 978 0 580 64047 6Amendments/corrigenda issued since publicationDate CommentsBS EN 1014-4:2010National forewordThis British Standard is the UK implementation of EN 1014-4:2010. Itsupersedes BS EN 1014-4:19

3、96 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee B/515, Wood preservation.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a co

4、ntract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS EN 1014-4:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1014-4 June 2010 ICS 71.100.50 Supersedes EN 1014-4:1995English Version Wood preservatives -

5、 Creosote and creosoted timber - Methods of sampling and analysis - Part 4: Determination of the water-extractable phenols content of creosote Produits de prservation du bois - Crosote et bois crosot - Mthodes dchantillonnage et danalyse - Partie 4 : Dtermination de la teneur en phnols extractibles

6、leau de la crosote Holzschutzmittel - Kreosot (Teerimprgnierl) und damit imprgniertes Holz - Probenahme und Analyse - Teil 4: Bestimmung des Gehaltes an wasserextrahierbaren Phenolen im Kreosot This European Standard was approved by CEN on 12 May 2010. CEN members are bound to comply with the CEN/CE

7、NELEC 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 CEN Management Centre or to a

8、ny 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 CEN Management Centre has the same status as the official versions

9、. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

10、ia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN nat

11、ional Members. Ref. No. EN 1014-4:2010: EBS EN 1014-4:2010EN 1014-4:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Preparation of the calibration solutions and of the test samples 66.1 Preparation of calibration solutions 66.2 Preparatio

12、n of the test sample .66.2.1 General 66.2.2 Preparation of “large“ test samples.66.2.3 Preparation of “small“ test samples 67 Procedure .78 Calculation 79 Expression of results 710 Precision .810.1 Repeatability .810.2 Reproducibility .811 Test report 8Annex A (informative) Example of chromatogram .

13、9Annex B (informative) Interpretation of the test results . 10Bibliography . 11BS EN 1014-4:2010EN 1014-4:2010 (E) 3 Foreword This document (EN 1014-4:2010) has been prepared by Technical Committee CEN/TC 38 “Durability of wood and wood-based products”, the secretariat of which is held by AFNOR. Thi

14、s European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2010, and conflicting national standards shall be withdrawn at the latest by December 2010. Attention is drawn to the possibility that some of

15、 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. This document supersedes EN 1014-4:1995. This standard forms part of a series of standards relating to the sampling and analysis of creo

16、sote and creosoted timber. The other standards of the series are: EN 1014-1, Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 1: Procedure for sampling creosote EN 1014-2, Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 2:

17、Procedure for obtaining a sample of creosote from creosoted timber for subsequent analysis EN 1014-3, Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 3: Determination of the benzo(a)pyrene content of creosote According to the CEN/CENELEC Internal Regulations, t

18、he national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nethe

19、rlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 1014-4:2010EN 1014-4:2010 (E) 4 1 Scope This European Standard specifies a high performance liquid chromatographic (HPLC) method for the determination of the water-extractable phen

20、ols content of creosote. For reasons of precision, this standard is applicable to the determination of the water-extractable phenols content of creosotes containing more than 10 g of water-extractable phenols per kilogram of creosote. 2 Normative references The following referenced documents are ind

21、ispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3

22、696:1987) 3 Principle The creosote sample is extracted with water. The aqueous extract is analyzed using high performance chromatography (HPLC) at constant temperature with a reversed phase packed column and isocratic elution. The result is compared with that from a known reference standard containi

23、ng various phenols known to be extracted by water from creosote. 4 Reagents 4.1 Acetonitrile HPLC grade. 4.2 Water according to grade 1 of EN ISO 3696:1995. 4.3 Methanol HPLC grade. 4.4 Acetic acid, HPLC grade. 4.5 Phenol purity 98 % (m/m) minimum. 4.6 2-methylphenol (o-cresol) purity 98 % (m/m) min

24、imum. 4.7 3-methylphenol (m-cresol) purity 98 % (m/m) minimum. 4.8 4-methylphenol (p-cresol) purity 98 % (m/m) minimum. 4.9 1,2-dihydroxybenzene (catechol) purity 98 % (m/m) minimum. 4.10 1,3-dihydroxybenzene (resorcinol) purity 98 % (m/m) minimum. 4.11 1,4-dihydroxybenzene (hydroquinone) purity 98

25、% (m/m) minimum. 4.12 2,4-dimethylphenol purity 98 % (m/m) minimum. 4.13 2,6-dimethylphenol purity 98 % (m/m) minimum. 4.14 3,5-dimethylphenol purity 98 % (m/m) minimum. BS EN 1014-4:2010EN 1014-4:2010 (E) 5 4.15 Acetonitrile/methanol mixture. Add 500 ml of acetonitrile (4.1) to 500 ml methanol (4.3

26、) and mix thoroughly. 4.16 Water/acetic acid mixture. Add 10 ml of acetic acid (4.4) to 990 ml water (4.2) and mix thoroughly. 4.17 HPLC eluent. Add together 180 ml acetonitrile (4.1), 180 ml methanol (4.3) and 640 ml of the water/acetic acid mixture (4.16), and mix thoroughly. NOTE If the HPLC equi

27、pment has a solvent mixing system where separate containers can hold the acetonitrile, the methanol, and the water/acetic acid mixture, the preparation of 4.17 is unnecessary. 4.18 Standard phenols solution. Weigh 200,0 mg to within 0,1 mg of each of the phenols (4.5 to 4.14) into a single 100 ml on

28、e-mark volumetric flask. Add 36 ml of the acetonitrile/methanol mixture (4.15). Make up to the mark with the water/acetic acid mixture (4.16). Transfer the solution to brown glass storage flasks (5.6). Store the flasks in the dark below 10 C. WARNING Care should be taken to avoid any skin contact wi

29、th the phenols. NOTE Under these storage conditions the solution is stable for six months although frequent use may result in faster ageing. 5 Apparatus Usual laboratory apparatus and glassware together with the following: 5.1 Volumetric glassware, which shall have an accuracy of at least 0,5 %. 5.2

30、 Single marked pipettes of 5 ml, 10 ml and 25 ml capacity. 5.3 High performance liquid chromatograph (HPLC) which shall consist of: a solvent delivery pump with constant flow regulation; 10 l loop injector; reversed phase stainless steel column, 250 mm in length with an internal diameter of 4 mm; pa

31、cked with C18 bonded silica stationary phase, having a particle size of 5 m; ultraviolet detector capable of being set at an absorption wavelength of 276 nm; an integrator or potentiometric recorder. NOTE As an alternative, any other HPLC configuration giving at least the same resolution (see Annex

32、A) could be used. 5.4 Analytical balance, capable of weighing to 0,1 mg. 5.5 Laboratory balance, capable of weighing to 0,1 g. 5.6 Brown glass storage flasks, of 100 ml capacity, fitted with ground glass stoppers. When only very small amounts of creosote (a few grams) are available, the following ad

33、ditional apparatus is necessary. 5.7 Glass screw-topped phial of 10 ml capacity. BS EN 1014-4:2010EN 1014-4:2010 (E) 6 5.8 Phase separation one-side silicone-treated filter papers, with a diameter of 70 mm1). 5.9 Glass syringe of 1 ml capacity. 6 Preparation of the calibration solutions and of the t

34、est samples 6.1 Preparation of calibration solutions Transfer by pipette (5.2) 25 ml, 10 ml and 5 ml of the standard phenols solution (4.18) to a series of 100 ml one-mark volumetric flasks. Make up to the mark with HPLC eluent (4.17). Transfer the calibration solutions to brown glass storage flasks

35、 (5.6). Store the flasks in the dark below 10 C. The calibration solutions should be prepared each day. 6.2 Preparation of the test sample 6.2.1 General Prepare duplicate test samples. Ensure that the sample of creosote consists of a single phase. If the laboratory sample derives from creosote in wh

36、ich crystals appear at ambient temperatures, heat the sample to a temperature at which it forms a single phase. 6.2.2 Preparation of “large“ test samples NOTE 1 This procedure should be followed if a sufficient amount of creosote (e.g. 250 g) is available. Weigh accurately and directly into a 500 ml

37、 separating funnel 100,0 g to within 1 mg of the creosote sample. Add the same amount of water (4.2) weighed to an accuracy of 0,1 g. Stopper the funnel and agitate it vigorously for 15 min, venting the funnel from time to time. Allow to stand until the two layers separate (approximately 10 min). Fi

38、lter the aqueous layer through a filter paper until it is clear. NOTE 2 Several passes through the filter paper may be required. Weigh 5,0 g of the clear aqueous extract to an accuracy of 0,01 g into a 10 ml one-mark volumetric flask. Make up to the mark with water (4.2) to produce the test sample.

39、NOTE 3 It may be necessary to use a larger quantity of the clear aqueous extract if the phenolic content is very low. 6.2.3 Preparation of “small“ test samples NOTE This procedure should be followed in case only a small amount of creosote (e.g. 2 g to 5 g) is available. Weigh accurately and directly

40、 into the screw-topped phial (5.7) 1 g of the creosote sample to an accuracy of 1 mg. Add twice this amount of water (4.2), weighed to an accuracy of 0,02 g, agitate vigorously for 15 min. Filter on the phase separation filter (5.8). Take approximately 1 ml of the aqueous phase retained on the filte

41、r with the syringe (5.9), taking care not to include any creosote. 1) Whatman 1 PS is an example of a suitable product available commercially. The information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. BS EN 1014-4:2

42、010EN 1014-4:2010 (E) 7 7 Procedure 7.1 Set up the apparatus (5.3) in accordance with the manufacturers instructions. Adjust the UV detector to a wavelength of 276 nm. 7.2 Under isocratic conditions set the flow rate through the column to 1,0 ml/min using the HPLC eluent (4.17). 7.3 Analyze the test

43、 samples and calibration solutions at the same temperature ( 0,5 C). Inject successively the series of calibration solutions and then the two test samples into the chromatograph (5.3). 7.4 Repeat 7.3 in reverse order by successively injecting portions of the two test samples followed by the calibrat

44、ion solutions. 7.5 Measure the height of the peaks for each individual phenol. 8 Calculation Calculate the content of each individual phenol in the two test samples (Pi1and Pi2) in grams phenol per kilogram creosote, using the equation: 0001ccsci=HCHPP where Pcis the concentration of the phenol cons

45、idered in the calibration solution nearest to the test sample, in milligrams per litre (mg/l); Hcis the mean of the duplicated peak heights of the phenol considered, obtained with the calibration solution, in millimetres (mm); Ccis the concentration of the aqueous extract of creosote in the test sam

46、ple (6.2), in milligrams per litre (mg/l); Hsis the peak height for the phenol under consideration obtained for the test sample (6.2), in millimetres (mm). Calculate the total water-extractable phenols content in the two test samples (Ps1and Ps2)in grams per kilogram of the laboratory sample, using

47、the following equation: i1s1PP = and i2s2PP = 9 Expression of results Report the water-extractable phenols content P, of the laboratory sample as the average Ps1and Ps2 in grams phenols per kilogram creosote, rounded to the nearest 1 g/kg. BS EN 1014-4:2010EN 1014-4:2010 (E) 8 10 Precision NOTE The

48、precision data are derived from an inter-laboratory test with “large“ test samples (6.2.1). The modifications introduced for “small“ test samples (6.2.2) imply that the precision might be lower than given in 10.1 and 10.2. 10.1 Repeatability Duplicate results obtained by the same operator shall be c

49、onsidered suspect if they differ by more than 5 % of the smaller. 10.2 Reproducibility Single results obtained by two laboratories shall be considered suspect if they differ by more than 15 % of the smaller. 11 Test report The test report shall include at least the following information: a) the number and date of this European Standard; b) full identification of the sample tested and details of its preparation for analysis; c) the date of th