1、BSI Standards PublicationBS EN 16453:2014Pulp, paper and paperboard Determination of phthalatesin extracts from paper andpaperboardBS EN 16453:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 16453:2014.The UK participation in its preparation was entrusted t
2、o TechnicalCommittee CW/47/3, Paper and board in contact with food.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication
3、. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 79012 6ICS 67.250; 85.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committe
4、e on 31 January 2014.Amendments issued since publicationDate Text affectedBS EN 16453:2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16453 January 2014 ICS 67.250; 85.060 English Version Pulp, paper and paperboard - Determination of phthalates in extracts from paper and paperboard Ptes, pa
5、pier et carton - Dosage des phtalates dans des extraits de papier et carton Zellstoff, Papier und Karton - Bestimmung von Phthalaten in Papier- und Kartonextrakten This European Standard was approved by CEN on 9 November 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations
6、 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-CENELEC Management Centre or to any CEN member. Thi
7、s 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-CENELEC Management Centre has the same status as the official versions. CEN memb
8、ers 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, Portug
9、al, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any for
10、m and by any means reserved worldwide for CEN national Members. Ref. No. EN 16453:2014 EBS EN 16453:2014EN 16453:2014 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Principle 5 3.1 General 5 3.2 Interferences 5 4 Materials .5 4.1 General 5 4.2 Pasteur pipettes .6 4.3 Double mark
11、 glass pipette of 0,05 ml, 0,2 ml, 0,5 ml, 1 ml, 5 ml and 10 ml .6 4.4 Volumetric flasks of 5 ml, 10 ml, 50 ml and 100 ml 6 4.5 Screw-cap glass bottle PYREX of 250 ml with a Polytetrafluorethylene-septa cap .6 4.6 Graduated cylinder of 200 ml .6 4.7 Round flask of 50 ml and 250 ml 6 4.8 Glass funnel
12、 .6 4.9 Polytetrafluorethylene-screw-cap glass vial single use (capacity adapted to the volume of concentrate) .6 5 Apparatus .6 5.1 Balance: capable of accurately weighing 0,000 1 g .6 5.2 Round flask heater.6 5.3 Rotary vacuum evaporator .6 5.4 Gas chromatograph coupled to a mass spectrometer (GC-
13、MS) .6 6 Reagents .6 6.1 General 6 6.2 Operating gases for gas chromatography/mass spectrometry, of high purity and in accordance with manufacturers specifications.6 6.3 Ethyl acetate, C4H8O2, CAS N 141-78-6 6 6.4 Isooctane, C8H18,CAS N 540-84-1 .6 6.5 Internal standard stock solution: For example d
14、4-ring-deuterated-dibutyl phthalate (D4-ring-DBP) at 10 g/l 6 6.6 Stock solutions of individual phthalate at 1 000 mg/l in ethyl acetate .7 7 Sampling .7 8 Preparation of the test sample of water extract .8 9 Preparation of the test sample of the organic solvent extract 8 10 Preparation of the test
15、sample of the MPPO Extract .8 11 Procedure .8 11.1 GC conditions 8 11.2 Calibration 9 11.3 Analysis of test samples .9 12 Expression of results . 10 12.1 For organic solvent extract: Expression of results. 10 12.2 For MPPO extract: Expression of results . 10 13 Test report . 10 14 Precision data . 1
16、1 Annex A (informative) GC-MS total ion chromatogram of a standard calibration solution of 2 mg/l of phthalates 12 BS EN 16453:2014EN 16453:2014 (E) 3 Foreword This document (EN 16453:2014) has been prepared by Technical Committee CEN/TC 172 “Pulp, paper and board”, the secretariat of which is held
17、by DIN. 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 July 2014, and conflicting national standards shall be withdrawn at the latest by July 2014. Attention is drawn to the possibility that some
18、 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. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to imple
19、ment this European Standard: 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,
20、 Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16453:2014EN 16453:2014 (E) 4 1 Scope This European Standard specifies an analytical test method for the determination of phthalates in water, solvent and modified polyphenylene oxide (MPPO) extracts of paper and b
21、oard materials and articles intended for food contact using gas chromatography coupled to mass spectrometry (GC-MS). This method is applicable to the determination of phthalates in concentration ranging from 0,025 mg/l to 0,5 mg/l for water and solvent extracts and 0,002 mg/dm2to 0,040 mg/dm2for MPP
22、O migration depending on the individual substance, the specified volume used for analysis and the value of the blank. Table 1 Phthlates determined by this method Name Abbreviation Formula CAS N Structure Diisobutyl-phthalate DIBP C16H22O484695 Dibutyl-phthalate DBP C16H22O484742 Di-(-ethylhexyl)-pht
23、halate DEHP C24H38O4117817 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
24、cument (including any amendments) applies. EN 645, Paper and board intended to come into contact with foodstuffs - Preparation of a cold water extract EN 647, Paper and board intended to come into contact with foodstuffs - Preparation of a hot water extract EN 14338, Paper and board intended to come
25、 into contact with foodstuffs - Conditions for determination of migration from paper and board using modified polyphenylene oxide (MPPO) as a simulant EN 15519, Paper and board intended to come into contact with foodstuffs - Preparation of an organic solvent extract EN 27213, Pulps - Sampling for te
26、sting (ISO 7213) EN ISO 186, Paper and board - Sampling to determine average quality (ISO 186) EN ISO 536, Paper and board - Determination of grammage (ISO 536) EN ISO 638, Paper, board and pulps - Determination of dry matter content - Oven-drying method (ISO 638) BS EN 16453:2014EN 16453:2014 (E) 5
27、 EN ISO 18856, Water quality - Determination of selected phthalates using gas chromatography/mass spectrometry (ISO 18856) 3 Principle 3.1 General Phthalates in the test extract from paper and board materials are determined by gas chromatography / mass spectrometry. The test extract is prepared from
28、 water, organic solvent and/or MPPO simulant according to respectively: EN 645, EN 647, EN 15519, EN 14338. Other phthalates, as listed in Table 1, may also be analysed by this procedure but it is necessary to determine its applicability in each case. 3.2 Interferences Due to their use as plasticize
29、r agents, phthalates are ubiquitous. Therefore, pay special attention to avoid any contamination. In order to avoid interferences and cross contamination, do not use plastics materials (tubes etc.). Cross contamination is likely to occur with laboratory air. Therefore, remove as far as possible, pla
30、stic materials from the laboratory. Cleaning agents often contain phthalates and may severely contaminate the laboratory air if in use regularly. Therefore, refrain from using these agents during application of this procedure. Phthalates may bleed from the septa of the injector port into the gas chr
31、omatograph, therefore use septa that are not likely to contaminate the system. Fittings of syringes or equipment and septa of the sampling bottles may as well contain phthalates. 4 Materials 4.1 General Common laboratory glassware, rinsed with ethyl acetate before use. After rinsing the glassware wi
32、th solvent, let residual solvent evaporate under a fume hood. In case of contamination, special attention should be paid to the volumetric flasks cleaning. For example the non-volumetric glassware could be cleaned in a furnace at 500C for at least 6 h. Glassware for volumetric purpose can change its
33、 properties due to the heating process and so should not be treated thus. Phthalates are ubiquitous laboratory contaminants. Each lot of reagent used for this method should be checked for phthalates contamination. BS EN 16453:2014EN 16453:2014 (E) 6 4.2 Pasteur pipettes 4.3 Double mark glass pipette
34、 of 0,05 ml, 0,2 ml, 0,5 ml, 1 ml, 5 ml and 10 ml 4.4 Volumetric flasks of 5 ml, 10 ml, 50 ml and 100 ml 4.5 Screw-cap glass bottle PYREX1)of 250 ml with a Polytetrafluorethylene-septa cap 4.6 Graduated cylinder of 200 ml 4.7 Round flask of 50 ml and 250 ml 4.8 Glass funnel 4.9 Polytetrafluorethylen
35、e-screw-cap glass vial single use (capacity adapted to the volume of concentrate) 5 Apparatus 5.1 Balance: capable of accurately weighing 0,000 1 g 5.2 Round flask heater 5.3 Rotary vacuum evaporator 5.4 Gas chromatograph coupled to a mass spectrometer (GC-MS) 6 Reagents 6.1 General Use as far as av
36、ailable reagents of analytical quality or better. Use only reagents with negligibly low concentrations of phthalates and verify by blank determinations. 6.2 Operating gases for gas chromatography/mass spectrometry, of high purity and in accordance with manufacturers specifications 6.3 Ethyl acetate,
37、 C4H8O2, CAS N 141-78-6 6.4 Isooctane, C8H18,CAS N 540-84-1 Store the following solutions in glass bottles at 18 C, protected from light. 6.5 Internal standard stock solution: For example d4-ring-deuterated-dibutyl phthalate (D4-ring-DBP) at 10 g/l 6.5.1 General Weigh for example, approximately 0,1
38、g with an accuracy of 0,001 g of d4-DBP in a 10 ml volumetric flask (4.4) and bring to volume with ethyl acetate (6.3). 1) PYREX is an example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an end
39、orsement by CEN of this product. BS EN 16453:2014EN 16453:2014 (E) 7 6.5.2 Solution A of internal standard at 100 mg/l in ethyl acetate Transfer 1 ml of the solution (6.5.1) into a 100 ml volumetric flask (4.4) and dilute to the mark with the ethyl acetate (6.3). 6.5.3 Solution B of internal standar
40、d at 10 mg/l in ethyl acetate Transfer 0,5 ml of the solution A (6.5.2) into a 5 ml volumetric flask (4.4) and dilute to the mark with the ethyl acetate (6.3). 6.5.4 Solution C of internal standard at 0,5 mg/l in ethyl acetate Transfer 0,25 ml of the stock solution A (6.5.2) into a 50 ml volumetric
41、flask (4.4) and dilute to the mark with the ethyl acetate (6.3). 6.6 Stock solutions of individual phthalate at 1 000 mg/l in ethyl acetate 6.6.1 General In a 100 ml volumetric flask (4.4), weigh approximately 0,1 g with an accuracy of 0,001 g of each of the reference substances and bring to volume
42、with ethyl acetate (6.3). 6.6.2 Intermediate solution of phthalates at 50 mg/l in ethyl acetate Transfer 5 ml of each stock solution (6.6.1) into a 100 ml volumetric flask (4.4) and dilute to the mark with ethyl acetate (6.3). 6.6.3 Calibration standard solutions of phthalates in isooctane Five stan
43、dard solutions are prepared by transferring respectively: 0,05 ml, 0,1 ml, 0,2 ml, 0,5 ml and 1 ml of the Intermediate solution (6.6.2) in 10 ml volumetric flasks (4.4) and 0,5 ml of the solution B of internal standard (6.5.3) by adjusting the volume with the solvent used for the extract of paper an
44、d board, for the preparation of solution having respectively concentrations of about: 0,25 mg/l, 0,5 mg/l, 1 mg/l, 2,5 mg/l and 5 mg/l of phthalate, and 0,5 mg/l of Internal Standard stock solution in each calibration solution. 6.6.4 Individual solutions of phthalates in ethyl acetate 1 mg/l for det
45、ermination of GC retention times Transfer 0,1 ml of stock solution (6.6.1) into a 100 ml volumetric flask (4.4) and dilute to the mark with ethyl acetate (6.3). 7 Sampling If the analysis is being made to evaluate a lot of paper, board or pulp, the sample shall be selected in accordance with EN ISO
46、186 or EN 27213, as relevant. If the analysis is made on another type of sample, report the source of the sample, and, if possible, the sampling procedure. Select the specimens so that they are representative of the sample received. If required, take a separate sample for the determination of the gr
47、ammage in accordance with EN ISO 536 and/or for the determination of dry matter content with EN ISO 638. For any storage or transport between sampling and analysis, protect the sample from contamination by using for example aluminium foil to over-wrap BS EN 16453:2014EN 16453:2014 (E) 8 8 Preparatio
48、n of the test sample of water extract The water extract of paper or board samples shall be carried out in accordance with EN 645 or EN 647. Every extraction test should be done in duplicate. In parallel, perform a blank analysis. The determination of the phthalates in the water extract shall be carr
49、ied out in accordance to EN ISO 18856. 9 Preparation of the test sample of the organic solvent extract The organic solvent extract of paper or board samples shall be carried out in accordance with EN 15519. The preferred solvent is isooctane but other solvents can also be used. Every extraction test should be done in duplicate before the determination described here. A specified volume of the solvent extract is taken2). 2 ml of solution C of Internal Standard is added to the organic solvent extract. It is then concentrated in a rotary vacuum evaporator until a
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