DIN EN 1014-4-2010 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、November 2010 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 71.100.50!$l1z“1731487www.din.deDDIN EN 1014-4Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 4: Determination of thewater-extractable phenols content of creosoteEnglish translation of DIN EN 1014-4:2010-11Holzschutzmittel Kreosot (Teerimprgnierl) und damit i

3、mprgniertes Holz Probenahme und Analyse Teil 4: Bestimmung des Gehaltes an wasserextrahierbarenPhenolen im KreosotEnglische bersetzung von DIN EN 1014-4:2010-11Produits de prservation du bois Crosote et bois crosot Mthodes dchantillonnage et danalyse Partie 4: Dtermination de la teneur enphnols extr

4、actibles leau de la crosoteTraduction anglaise de DIN EN 1014-4:2010-11SupersedesDIN EN 1014-4:1995-09www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1310.10 DIN EN 1014-4:2010-11 2 A comma is used as the decimal marker. National f

5、oreword This standard has been prepared by Technical Committee CEN/TC 38 “Durability of wood and wood-based products” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was the Normenausschuss Holzwirtschaft und Mbel (Timber and Furniture Standards Committee), Work

6、ing Committee NA 042-03-06 AA Spiegelausschuss zu CEN/TC 38 und ISO/TC 165/SC 1 Dauerhaftigkeit von Holz und Holzprodukten. The DIN Standard corresponding to the International Standard referred to in this document is as follows: EN ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN 1

7、014-4:1995-09 as follows: a) the standard has been editorially revised. Previous editions DIN EN 1014-4: 1995-09 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1014-4 J

8、une 2010 ICS 71.100.50 Supersedes EN 1014-4:1995English Version Wood preservatives - 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 dchant

9、illonnage et danalyse - Partie 4 : Dtermination de la teneur en phnols extractibles 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

10、 was approved by CEN on 12 May 2010. 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 na

11、tional standards may be obtained on application to the CEN 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 an

12、d notified to the CEN Management Centre has the same status as the official versions. 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,

13、 Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, 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 Al

14、l rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1014-4:2010: EEN 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 tes

15、t samples 66.1 Preparation of calibration solutions 66.2 Preparation 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 Reproducibilit

16、y .811 Test report 8Annex A (informative) Example of chromatogram .9Annex B (informative) Interpretation of the test results . 10Bibliography . 11DIN EN 1014-4:2010-11 EN 1014-4:2010 (E) 3 Foreword This document (EN 1014-4:2010) has been prepared by Technical Committee CEN/TC 38 “Durability of wood

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

18、est by December 2010. 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. This document supersedes EN 1014-4:1995. This standard forms par

19、t of a series of standards relating to the sampling and analysis of creosote 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

20、 Creosote and creosoted timber Methods of sampling and analysis Part 2: 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

21、content of creosote According to the CEN/CENELEC Internal Regulations, the 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, Hunga

22、ry, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 1014-4:2010-11 EN 1014-4:2010 (E) 4 1 Scope This European Standard specifies a high performance liquid chro

23、matographic (HPLC) method for the determination of the water-extractable phenols 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 o

24、f creosote. 2 Normative references The following referenced documents are indispensable 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 3696:19

25、95, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 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 eluti

26、on. The result is compared with that from a known reference standard containing 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 p

27、urity 98 % (m/m) minimum. 4.6 2-methylphenol (o-cresol) purity 98 % (m/m) minimum. 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) p

28、urity 98 % (m/m) minimum. 4.11 1,4-dihydroxybenzene (hydroquinone) purity 98 % (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. DIN EN 1014-4:2010-11 EN 1014-4:2010 (E) 5 4.15 Aceto

29、nitrile/methanol mixture. Add 500 ml of acetonitrile (4.1) to 500 ml methanol (4.3) 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

30、of the water/acetic acid mixture (4.16), and mix thoroughly. NOTE If the HPLC equipment 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,

31、0 mg to within 0,1 mg of each of the phenols (4.5 to 4.14) into a single 100 ml one-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

32、 in the dark below 10 C. WARNING Care should be taken to avoid any skin contact with 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 follow

33、ing: 5.1 Volumetric glassware, which shall have an accuracy of at least 0,5 %. 5.2 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 ph

34、ase stainless steel column, 250 mm in length with an internal diameter of 4 mm; packed 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 alterna

35、tive, any other HPLC configuration giving at least the same resolution (see Annex 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

36、 only very small amounts of creosote (a few grams) are available, the following additional apparatus is necessary. 5.7 Glass screw-topped phial of 10 ml capacity. DIN EN 1014-4:2010-11 EN 1014-4:2010 (E) 6 5.8 Phase separation one-side silicone-treated filter papers, with a diameter of 70 mm1). 5.9

37、Glass syringe of 1 ml capacity. 6 Preparation of the calibration solutions and of the test 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 wi

38、th HPLC eluent (4.17). Transfer the calibration solutions to brown glass storage flasks (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 cr

39、eosote consists of a single phase. If the laboratory sample derives from creosote in which 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 am

40、ount of creosote (e.g. 250 g) is available. Weigh accurately and directly into a 500 ml 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 fro

41、m time to time. Allow to stand until the two layers separate (approximately 10 min). Filter 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-m

42、ark volumetric flask. Make up to the mark with water (4.2) to produce the test sample. 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

43、 small amount of creosote (e.g. 2 g to 5 g) is available. Weigh accurately and directly 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 sepa

44、ration filter (5.8). Take approximately 1 ml of the aqueous phase retained on the filter 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

45、 Standard and does not constitute an endorsement by CEN of this product. DIN EN 1014-4:2010-11 EN 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 f

46、low rate through the column to 1,0 ml/min using the HPLC eluent (4.17). 7.3 Analyze the test 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 rever

47、se order by successively injecting portions of the two test samples followed by the calibration 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 c

48、reosote, using the equation: 0001ccsci=HCHPP where Pcis the concentration of the phenol considered 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

49、 millimetres (mm); Ccis the concentration of the aqueous extract of creosote in the test sample (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 the following equation: