DIN EN 1014-3-2010 Wood preservatives - Creosote and creosoted timber - Methods of sampling and analysis - Part 3 Determination of the benzo(a)pyrene content of creosote German ver.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!$l1u“1731482www.din.deDDIN EN 1014-3Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 3: Determination of thebenzo(a)pyrene content of creosoteEnglish translation of DIN EN 1014-3:2010-11Holzschutzmittel Kreosot (Teerimprgnierl) und damit imprgniertes

3、 Holz Probenahme und Analyse Teil 3: Bestimmung des Gehaltes an Benzo(a)pyren imKreosotEnglische bersetzung von DIN EN 1014-3:2010-11Produits de prservation du bois Crosote et bois crosot Mthodes d chantillonnage et danalyse Partie 3: Dtermination de la teneur enbenzoapyr ne dans la crosoteTraductio

4、n anglaise de DIN EN 1014-3:2010-11SupersedesDIN EN 1014-3:1997-11www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.14 10.10 DIN EN 1014-3:2010-11 2 A comma is used as the decimal marker. National foreword This standard has been prep

5、ared 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), Working Committee NA 042-03-06 AA Spieg

6、elausschuss 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 1014-3:1997-11 as follows: a) the st

7、andard has been editorially revised. Previous editions DIN EN 1014-3: 1995-12, 1997-11 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1014-3 June 2010 ICS 71.100.50 Sup

8、ersedes EN 1014-3:1997English Version Wood preservatives - Creosote and creosoted timber - Methods of sampling and analysis - Part 3: Determination of the benzo(a)pyrene content of creosote Produits de prservation du bois - Crosote et bois crosot - Mthodes dchantillonnage et danalyse - Partie 3: Dte

9、rmination de la teneur en benzoapyrne dans la crosote Holzschutzmittel - Kreosot (Teerimprgnierl) und damit imprgniertes Holz - Probenahme und Analyse - Teil 3: Bestimmung des Gehaltes an Benzo(a)pyren im Kreosot This European Standard was approved by CEN on 12 May 2010. CEN members are bound to com

10、ply 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 national standards may be obtained on application to the CEN Manage

11、ment 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 and notified to the CEN Management Centre has the same status as th

12、e 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, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romani

13、a, 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 All rights of exploitation in any form and by any means reserved wo

14、rldwide for CEN national Members. Ref. No. EN 1014-3:2010: EEN 1014-3:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .46 Preparation of the calibration solutions and of the test samples 56.1 Preparation of the calibration solutions 56.2 Prep

15、aration of the test samples .57 Procedure .68 Calculation 69 Expression of results 610 Precision .710.1 Repeatability .710.2 Reproducibility .711 Test report 7Annex A (informative) Examples of chromatograms .8Annex B (informative) Interpretation of the test results . 11Bibliography . 12DIN EN 1014-3

16、:2010-11 EN 1014-3:2010 (E) 3 Foreword This document (EN 1014-3:2010) has been prepared by Technical Committee CEN/TC 38 “Durability of wood and wood-based products”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publica

17、tion 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 the elements of this document may be the subject of patent rights. CEN and/or CENELEC

18、shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 1014-3:1997. This standard forms part 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 prese

19、rvatives 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: Procedure for obtaining a sample of creosote from creosoted timber for subsequent analy

20、sis EN 1014-4, Wood preservatives Creosote and creosoted timber Methods of sampling and analysis Part 4: Determination of the water-extractable phenols content of creosote According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to

21、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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden

22、, Switzerland and the United Kingdom. DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 4 1 Scope This European Standard specifies a method for the determination of benzo(a)pyrene in creosote using high performance liquid chromatography (HPLC). This standard is only applicable to creosotes containing more th

23、an 30 mg/kg benzo(a)pyrene. 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

24、. EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Principle The creosote sample is diluted to an appropriate concentration with an acetonitrile/water mixture. The diluted sample is analyzed using high performance liquid chromatography (HPLC) at

25、constant temperature with a reverse phase packed column and isocratic elution. The result is compared with that from a known reference standard. 4 Reagents 4.1 Acetonitrile water mixture. Add 220 ml of water (according to grade 1 of EN ISO 3696:1995) to 780 ml of acetonitrile (CH3CN, HPLC grade) and

26、 mix thoroughly. The mixture shall be at room temperature before use. 4.2 Benzo(a)pyrene solution, containing approximately 0,1 mg/ml of benzo(a)pyrene. Weigh to the nearest 0,1 mg, approximately 0,01 g of benzo(a)pyrene with a purity of min. 98 % and transfer it quantitatively to a 100 ml one-mark

27、volumetric flask. Add 50 ml of the acetonitrile (CH3CN, HPLC grade). Dissolve the benzo(a)pyrene and make up to the mark with the acetonitrile-water mixture (4.1). Store the prepared solution in the stoppered brown glass storage flasks (5.6) in the dark, at a temperature below 10 C. CAUTION Care sho

28、uld be taken to prevent benzo(a)pyrene contacting the skin. NOTE 1 Under normal conditions, this solution is stable for six months, although frequent use may result in faster ageing. NOTE 2 Commercially available certified standard solutions, including those containing additional components, may be

29、used. 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 Single mark pipettes class A of 1 ml, 2 ml, 5 ml and 20 ml capacity. DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 5 5.3 High performance l

30、iquid chromatograph (HPLC) which shall consist of a solvent delivery pump with constant flow regulation; on-line degasser; 20 l loop injector; reverse phase stainless steel column, 250 mm in length with an internal diameter of 4 mm, packed with C18 bonded silica stationary phase, having a particle s

31、ize of 5 m; the use of a column specially designed for polyaromatic hydrocarbons analysis is recommended; fluorescence detector capable of being set at (380 3) nm excitation wavelength and (403 5) nm emission wavelength; a potentiometric recorder. NOTE As an alternative, any other HPLC configuration

32、 giving at least the same resolution (see Figures A.1 and A.2 or A.3) could be used. 5.4 Analytical balance, capable of weighing to 0,1 mg. 5.5 Ultrasonic bath capable of containing a 100 ml volumetric flask. 5.6 Brown glass storage flasks of 100 ml capacity, fitted with ground glass stoppers. 5.7 G

33、lass or metal receptacles fitted with stoppers. 5.8 Glass syringe for HPLC, of 50 I capacity. 6 Preparation of the calibration solutions and of the test samples 6.1 Preparation of the calibration solutions Transfer by pipette (5.2) 1 ml of the benzo(a)pyrene solution (4.2) to a 100 ml one-mark volum

34、etric flask and dilute to the mark with the acetonitrile-water mixture (4.1). To a series of 100 ml one-mark volumetric flasks, transfer by pipette (5.2) 1 ml, 2 ml, 5 ml and 20 ml of this solution and dilute to the mark with acetonitrile-water mixture (4.1). This provides calibration solutions cont

35、aining 0,01 mg/I, 0,02 mg/I, 0,05 mg/I and 0,20 mg/I benzo(a)pyrene. Store the calibration solutions in stoppered brown glass storage flasks (5.6.) in the dark at a temperature below 10 C. NOTE Under normal conditions, the calibration solutions are stable for three months, although frequent use may

36、result in faster ageing. 6.2 Preparation of the test samples Prepare duplicate test samples. The laboratory sample shall be in a closed receptacle (5.7). Heat the closed receptacle to 70 C for (30 2) min to ensure that the sample is completely liquid. Weigh to the nearest 0,1 mg, 30,0 mg of the labo

37、ratory sample into a 100 ml one-mark volumetric flask. NOTE Attention should be paid that no re-crystallization occurs during this transfer. Record the masses taken as m1and m2. Add approximately 80 ml of the acetonitrile-water mixture (4.1). Place the volumetric flask in the ultrasonic bath (5.5) f

38、or 5 min to dissolve the sample. DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 6 When the sample has dissolved completely, make up to the mark with the acetonitrile-water mixture (4.1). 7 Procedure 7.1 Set-up the HPLC (5.3) in accordance with the manufacturers instructions. Adjust the fluorescence detect

39、or to the following wavelengths: excitation: (380 3) nm; emission: (403 5) nm. The fluorescence detector shall be fine-tuned to maximize the signal for benzo(a)pyrene. Under isocratic conditions set the flow rate through the column to 1,2 ml/min using the acetonitrile-water mixture (4.1) as the elue

40、nt. 7.2 Analyze the test samples and the calibration solutions at the same temperature ( 0,5 C). At the same temperature (i.e. within 0,5 C) and using the syringe (5.8) fill up the loop injector and inject successively the series of calibration solutions (6.1) and then the two test samples into the

41、HPLC apparatus (5.3). 7.3 Repeat 7.2 in reverse order by successively injecting portions of the two test samples followed by the calibration solutions. 7.4 Measure the peaks heights for benzo(a)pyrene produced by the HPLC recorder for all test samples and calibration solutions. 8 Calculation Calcula

42、te the benzo(a)pyrene content of the two samples, Bs1and Bs2, expressed in milligrams benzo(a)pyrene per kilogram creosote, using the equation: 6ccscs10=HCHBB where Bcis the concentration of the benzo(a)pyrene calibration solution nearest to the test sample in milligrams per litre (mg/l); Hcis the m

43、ean of the duplicated benzo(a)pyrene peak heights obtained with the calibration solution in millimetres (mm); Ccis the concentration of creosote in the test sample (6.2) in milligrams per litre (mg/l); Hsis the peak height obtained for the test sample (6.2) in millimetres (mm). 9 Expression of resul

44、ts Report the benzo(a)pyrene content B, of the laboratory sample as the average of Bs1 and Bs2in milligrams per kilogram benzo(a)pyrene in creosote, rounded to the nearest 1 mg/kg (see Annex B). DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 7 10 Precision 10.1 Repeatability Results obtained by the same o

45、perator shall be considered suspect if the duplicates differ by more than 10 % of the lower in the concentration range up to 100 mg/kg benzo(a)pyrene in creosote and 5 % of the lower above 100 mg/kg benzo(a)pyrene in creosote. 10.2 Reproducibility Single results obtained by two laboratories shall be

46、 considered suspect if they differ by more than 30 % of the lower. 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 o

47、f the test; d) the results of the analysis, expressed as milligrams per kilogram benzo(a)pyrene in creosote (see Clause 9); e) whether the repeatability has been verified; f) any particular points observed in the course of the test; g) any operations not specified in the method or regarded as option

48、al which might have affected the result. DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 8 Annex A (informative) Examples of chromatograms Column: Packing C 18-particle size 5 m; Length 250 mm; Internal diameter 4,6 mm. Operating conditions: Flow: 1,2 ml/min; Temperature: 25 C. NOTE Retention times depend

49、on the column used and on the operational conditions. Figure A.1 Standard solution DIN EN 1014-3:2010-11 EN 1014-3:2010 (E) 9 Column: Packing C 18-particle size 5 m; Length 250 mm; Internal diameter 4,6 mm. Operating conditions: Flow: 1,2 ml/min; Temperature: 25 C. NOTE Retention times depend on the column used and on the operational conditions. Figure A.2 Creosote oil with approximately 500 mg