1、BS EN ISO6401:2008ICS 83.080.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Poly(vinylchloride) Determination ofresidual vinyl chloridemonomer Gas-chromatographicmethod (ISO 6401:2008)This British Standard was published under theauthority of the Stan
2、dardsPolicy and StrategyCommittee on 32008 BSI 2008ISBN 978 0 580 57207 4Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 6401:2008National forewordThis British Standard is the UK implementation of EN ISO 6401:2008. Itsupersedes BS EN ISO 6401:2004 which is withdrawn.The UK parti
3、cipation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.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 contract. Users are responsible f
4、or its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.0 NovemberEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 6401September 2008ICS 83.080.20 Supersedes EN ISO 6401:2004 English VersionPlastics - Poly(vinyl chloride) - Determination of res
5、idual vinylchloride monomer - Gas-chromatographic method (ISO6401:2008)Plastiques - Poly(chlorure de vinyle) - Dtermination duchlorure de vinyle monomre rsiduel - Mthode parchromatographie en phase gazeuse (ISO 6401:2008)Kunststoffe - Polyvinylchlorid - Bestimmung desRestgehaltes an Vinylchlorid-Mon
6、omer -Gaschromatographisches Verfahren (ISO 6401:2008)This European Standard was approved by CEN on 16 August 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any a
7、lteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 tr
8、anslationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany
9、, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagem
10、ent Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 6401:2008: EBS EN ISO 6401:2008EN ISO 6401:2008 (E) 3 Foreword This document (EN ISO 6401:2008) has been prepared by Technical C
11、ommittee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. 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 March 2009, a
12、nd conflicting national standards shall be withdrawn at the latest by March 2009. 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
13、 document supersedes EN ISO 6401:2004. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gre
14、ece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 6401:2008 has been approved by CEN as a EN ISO 6401:2008 without any
15、modification. BS EN ISO 6401:2008ISO 6401:2008(E) ISO 2008 All rights reserved iiiContents Page1 Scope 12 Normative references 13 Terms and definitions 14 Principle 15 Sampling . 16 Apparatus . 27 Reagents and materials 28 Procedure . 39 Calculation . 410 Precision . 411 Test report 4Annex A (inform
16、ative) Suitable GC columns for the determination of vinyl chloride monomer . 5Annex B (informative) Typical responses for vinyl chloride monomer calibration solutions . 6BS EN ISO 6401:2008ISO 6401:2008(E)iv ISO 2008 All rights reservedForewordISO (the International Organization for Standardization)
17、 is a worldwide federation of national standards bodies(ISO member bodies). The work of preparing International Standards is normally carried out through ISOtechnical committees. Each member body interested in a subject for which a technical committee has beenestablished has the right to be represen
18、ted on that committee. International organizations, governmental andnon-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the InternationalElectrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are draft
19、ed in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standardsadopted by the technical committees are circulated to the member bodies for voting. Publication as anInternational Standar
20、d requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of patentrights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 6401 was prepared by Techn
21、ical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemicalproperties.This second edition cancels and replaces the first edition (ISO 6401:1985), which has been technically revised.BS EN ISO 6401:2008INTERNATIONAL STANDARD ISO 6401:2008(E) ISO 2008 All rights reserved 1Plastics Poly(vin
22、yl chloride) Determination of residual vinyl chloride monomer Gas-chromatographic methodSAFETY PRECAUTIONS Persons using this document should be familiar with normal laboratorypractice, if applicable. This document does not purport to address all of the safety concerns, if any,associated with its us
23、e. It is the responsibility of the user to establish appropriate safety and healthpractices and to ensure compliance with any regulatory requirements.1ScopeThis International Standard specifies a method for the determination of vinyl chloride monomer in homopolymerand copolymer resins of vinyl chlor
24、ide and compounded materials. The method is based on sample dissolutionand headspace gas chromatography. Concentrations of vinyl chloride in the range to canbe determined.A “dry method”, suitable for PVC resins but not compounded materials, is widely used within the industry forin-house determinatio
25、ns. A separate International Standard based on this methodology is under development.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of the
26、 referenced document(including any amendments) applies.ISO 472, Plastics Vocabulary3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 apply.4 PrincipleThe level of vinyl chloride monomer is determined by headspace gas chromatography of the polymer te
27、stsample dissolved/swollen in N,N-dimethylacetamide.5 SamplingA representative sample shall be taken.A concentration gradient may form in stored resin samples due to the volatility of vinyl chloride. Cooling of thesample prior to sampling is advisable but condensation of humidity must be avoided. Sa
28、mple preparation shallbe carried out as quickly as possible to minimize losses of residual monomer. When exchanging samplesbetween laboratories or when storage is necessary, samples should be sealed in completely filled and sealedglass bottles or vials (e.g. 6.5, 6.6).0,1 mg/kg 3,0 mg/kgBS EN ISO 64
29、01:2008ISO 6401:2008(E)2 ISO 2008 All rights reserved6 ApparatusStandard laboratory apparatus and the following:6.1 Gas chromatograph (GC), fitted with an automatic static headspace sampler.6.2 Flame ionization detector (FID).6.3 Gas-chromatographic column.The signal obtained with a solution contain
30、ing of vinyl chloride per litre shall be at least three times thatof the baseline noise. The limit of detection of the method is vinyl chloride in test samples. Examplesof suitable columns are described in Annex A, Table A.1.6.4 Data-processing system, for data acquisition and evaluation of GC runs.
31、6.5 Glass bottles, capacity , with polytetrafluoroethylene (PTFE) faced silicone septa and aluminiumcaps.6.6 Glass vials, capacity , with polytetrafluoroethylene (PTFE) faced silicone septa and aluminiumcaps.6.7 Crimping and decapping tools, for sealing and uncapping the vials.6.8 Glass pipettes, ca
32、pacity and .6.9 Microsyringes, capacity and .6.10 Gastight glass syringe, capacity , with lock valve.6.11 Analytical balance, capable of weighing to .7 Reagents and materialsAll reagents shall be of recognized analytical grade.WARNING Vinyl chloride is a hazardous substance which is a gas at ambient
33、 temperature. Thepreparation of solutions should therefore be carried out only under a well-ventilated fume hood.7.1 Vinyl chloride, of purity greater than . The vinyl chloride gas cylinder shall be fitted with a syringeadapter.7.2 N,N-dimethylacetamide, density . The solvent shall not contain any i
34、mpurity with thesame chromatographic retention time as vinyl chloride under the conditions of the test.WARNING N,N-dimethylacetamide is also a hazardous substance.7.3 Detector gases and carrier gas: High-purity gases shall be used to achieve the required low limits ofquantification.7.4 Vinyl chlorid
35、e, standard solution, with a vinyl chloride concentration of approximately .To a glass bottle (6.5), add, using a glass pipette (6.8), of N,N-dimethylacetamide (7.2) and cap thebottle with a PTFE-lined silicone septum. Weigh (to ) the bottle containing the N,N-dimethylacetamide.Introduce of vinyl ch
36、loride gas through the septum into the N,N-dimethylacetamide, using a pre-flushedgastight syringe (6.10) and holding the end of the syringe needle below the surface of the liquid. Avoid thecontents of the bottle becoming contaminated by air. Identify this solution as solution A.Repeat the procedure
37、with a second glass bottle and identify the resultant solution as solution B.0,01 mg0,1 mg/kg30 ml22,5 ml25 ml 10 ml500l 100l10 ml0,1 mg99,5 % = 0,937 g/ml1 600 mg/l30 ml 25 ml0,1 mg10 ml10 ml30 mlBS EN ISO 6401:2008ISO 6401:2008(E) ISO 2008 All rights reserved 3Leave both bottles for at room temper
38、ature to allow complete adsorption of the vinyl chloride. Reweigh to thenearest to determine the mass of monomer which has been added. The mass of vinyl chloride in eachstandard solution will be about , depending on cylinder pressure. Record the concentration of vinylchloride in solutions A and B in
39、 milligrams per litre.Store the solutions in a refrigerator.7.5 Vinyl chloride, working calibrant stock solutions, with a vinyl chloride concentration of approximately.To a glass bottle, add, using a glass pipette, of N,N-dimethylacetamide (7.2) and seal with aPTFE-lined silicone septum and cap. Tra
40、nsfer of solution A through the septum into the bottle using asuitable syringe.Repeat for solution B and label the two diluted calibrant solutions as solution C and solution D.Record the concentration of vinyl chloride in the working calibrant stock solutions in milligrams per litre.7.6 Vinyl chlori
41、de calibration solutions, with vinyl chloride concentrations between andapproximately .Take seven headspace vials (6.6) and add, using a glass pipette, of N,N-dimethylacetamide (7.2)to each. Using a syringe, transfer , , , , , and of solution C into theindividual vials and seal with silicone/PTFE se
42、pta and caps. Take two more headspace vials and addof N,N-dimethylacetamide. To these add of solution D (giving a final concentration of ) andseal with a septum and cap. These last two solutions are used as check solutions.8 Procedure8.1 Preparation of test solutionsWeigh of sample (to ) into a head
43、space vial (cut compounded materials into small pieces)and add of dimethylacetamide. Seal with a silicone/PTFE septum and then cap the vial. Repeat this toproduce triplicate test solutions for each sample.8.2 Gas chromatographyDepending on the type of gas chromatograph and column used for the determ
44、ination, establish the appropriateGC and FID parameters.NOTE For guidance, the transfer line temperature and column oven temperature profile established for a GC equipped withcolumn 2 described in Annex A are:Transfer line temperature: .Column oven temperature profile: Isothermal at for , from to at
45、 , then from toat . Under these conditions, vinyl chloride elutes at .8.3 DeterminationTransfer the test solutions, calibrant solutions and two check solutions to the static headspace sampler.Equilibrate them at for prior to analysis.Suggested operating parameters for the headspace sampler are:needl
46、e temperature: ;pressurizing time: ;2h0,1 mg40 mg32 mg/l30 ml 25 ml500l0 mg/l0,3 mg/l22,5 ml 10 ml100l 0l 20l 40l 50l 60l 80l 100l22,5 ml10 ml 20l 0,06 mg/l1g 0,1 mg 22,5 ml10 ml150C80C 2min 80C 170C 5C/min 170C230C 20C/min 8,4 min70C 1h150C1,0 minBS EN ISO 6401:2008ISO 6401:2008(E)4 ISO 2008 All ri
47、ghts reservedinjection time: ;withdrawal time: .8.4 Preparation of the calibration graphPlot a graph of the vinyl chloride contents of the calibration solutions, in milligrams per litre, against thecorresponding peak areas.9 CalculationDetermine the vinyl chloride content, in milligrams per litre, o
48、f the three test solutions and two check solutionsfrom the calibration graph.The vinyl chloride content of the sample, expressed in milligrams per kilogram, is given by the formulawhereis the vinyl chloride content, in milligrams per litre, of the test solution, determined from thecalibration graph;
49、is the mass, in grams, of vinyl chloride in the test solution.Confirm that the data obtained on the check solutions gives the concentration expected (within the repeatabilitycriterion for the method to be determined). If this is the case, report the results for each of the three testsolutions individually, as well as their arithmetic mean and the standard deviation from the mean.10 PrecisionTo be determined by interlaboratory trial.11 Test reportThe test report shall include the following informa
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