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1、BRITISH STANDARD BS EN 13628-1:2002 Packaging Flexible packaging material Determination of residual solvents by static headspace gas chromatography Part 1: Absolute methods The European Standard EN 13628-1:2002 has the status of a British Standard ICS 55.040 ? BS EN 13628-1:2002 This British Standar
2、d, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 21 October 2002 BSI 21 October 2002 ISBN 0 580 40627 X National foreword This British Standard i
3、s the official English language version of EN 13628-1:2002. The UK participation in its preparation was entrusted by Technical Committee PKW/5, Primary and transport packaging, to Subcommittee PKW/5/26, Packaging made from flexible materials, which has the responsibility to: A list of organizations
4、represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondenc
5、e Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itsel
6、f confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and pr
7、omulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 16, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publ
8、ication Amd. No. DateComments EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13628-1 October 2002 ICS 55.040 English version Packaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 1: Absolute methods Emballage - Matriaux demba
9、llages souples - Dtermination des solvants rsiduels par chromatographie en phase gazeuse et espace de tte statique - Partie 1: Mthodes absolues Verpackung - Flexible Packstoffe - Bestimmung der Restlsemittel durch statische Dampfraumanalyse mittels Gaschromatographie - Teil 1: Absolute Verfahren Thi
10、s European Standard was approved by CEN on 26 August 2002. 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 referen
11、ces concerning such national standards may be obtained on application to the 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 i
12、ts own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
13、 Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2002 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN natio
14、nal Members. Ref. No. EN 13628-1:2002 E EN 13628-1:2002 (E) 2 Contents page Foreword3 1Scope 4 2Normative references 4 3Principle4 4Reagents.4 5Apparatus .5 6Sampling.8 7Test specimens8 8Incubation of the test specimens.8 9Procedure .9 10Precision data.16 11Test report 16 EN 13628-1:2002 (E) 3 Forew
15、ord This document EN 13628-1:2002 has been prepared by Technical Committee CEN/TC 261 “Packaging“, 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 April
16、2003, and conflicting national standards shall be withdrawn at the latest by April 2003. This standard is part of a standard for determination of residual solvents by static headspace gas chromatography, which is published in two parts: - Part 1: Absolute methods - Part 2: Industrial methods Accordi
17、ng to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Por
18、tugal, Spain, Sweden, Switzerland and the United Kingdom. EN 13628-1:2002 (E) 4 1 Scope This part of this European Standard specifies methods for the quantitative determination of residual solvents in flexible packaging by static headspace chromatography where the chemical identities of the residual
19、 solvents to be determined are known before commencing the analysis. Residues from thermal decomposition products are not within the scope of this standard. The method is applicable to flexible packaging materials that may consist of mono- or multilayer plastic films, paper or board, foil or combina
20、tions thereof. This method does not apply to residual solvents with amounts lower than 0,5 mg/m. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, a
21、nd the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (
22、including amendments). ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. 3 Principle Specimens of the flexible packaging material are placed in a hermeti
23、cally closed vial and heated under closely controlled conditions of time and temperature to vaporize solvents into the headspace. The amount of solvent released into the headspace is determined by transferring an aliquot of the headspace into a gas chromatograph for analysis. The transfer may be per
24、formed: a) by specific semi-automatic or automatic systems which allow pressurization of the heated vials. Quantification is achieved by the multiple headspace extraction (MHE) procedure using external or internal standards; b) manually or automatically by using a heated gastight syringe or a loop w
25、ithout pressurization of the heated vials. Quantification is achieved by the standard addition method. NOTEA prerequisite for a quantitative determination of residual solvents by headspace gas chromatography is that a partition equilibrium for the solvent between the gas phase and the solid phase ha
26、s been reached before an aliquot of the headspace is withdrawn and transferred into the gas chromatograph. During the analysis, there may be interferences from possible products of thermal decomposition. Additional peaks due to these products shall not be considered for evaluation of residual solven
27、ts. 4 Reagents 4.1 General All reagents shall be of a recognized analytical reagent grade. NOTEGrades stated as being suitable for chromatography are commercially available and are recommended for use as reference for standard calibration solutions. Appropriate safety precautions should be used when
28、 handling toxic and/or flammable solvents. EN 13628-1:2002 (E) 5 4.2 Reference solvents, for the preparation of standard calibration solutions. 4.3 Dilution solvent, with a retention time different from those of residual solvents in the sample. NOTESolvents such as hexane, cyclohexanone, acid amides
29、 and glycerol triacetate (triacetin) are appropriate. 5 Apparatus 5.1 Glass vials, of capacity 6 ml, 8 ml, 20 ml, 50 ml or 100 ml depending upon the specific requirements of accessory equipment, for example, the headspace sampler, fitted with an inert septum seal and aluminium crimp tops. The septum
30、 seal shall neither absorb nor release volatile components, shall be gas tight during incubation and shall permit samples of the headspace gas to be withdrawn by syringe for subsequent analysis. NOTEElastomers lined with polytetrafluoroethylene (PTFE) are suitable materials for septum seals. 5.2 Cri
31、mping tool, for sealing the vials with the aluminium crimp tops. 5.3 Seal removing tool. 5.4 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.5 Template, for cutting samples. The dimensions of this template shall be matched to the vial volume used. 5.6 Scalpel or sharp knife. 5.7 Syr
32、inges (e.g. 1 l, 10 l). 5.8 Gas chromatograph, having a flame ionization detector or equivalent for the solvents to be determined. 5.9 Gas chromatographic column, either packed or capillary, that will give good resolution of the solvents to be determined from any other components that might be injec
33、ted with the specimen of the headspace. Examples for suitable columns and operation conditions are: a) Packed column: length: 3 m; internal diameter: 3,2 mm; column filling: 80/120 mesh graphitised carbon, deactivated with polyethyleneglycol; carrier gas: N2, 20 ml/min; injector temperature: 220 C;
34、temperature programme: 80 C; raised to 160 C at 6 C/min; raised to 225 C at 1,5 C/min; held for 16 min; NOTE 1A corresponding chromatogram obtained for a mixture of solvents is shown in Figure 1. EN 13628-1:2002 (E) 6 Key 14,23 methanol 26,67 ethanol 39,25 acetone 417, 06 ethyl acetate 519,1 butanol
35、 623,34 trichloroethylene 728,4 isobutyl acetate 833,87 methyl isobutylketone 941,86 toluene 1064.06 xylene ARetention time (min) BPeak height Figure 1 Example of chromatogram obtained with a packed column or b) Capillary column (fused silica): length: 30 m; internal diameter: 0,32 mm; stationary ph
36、ase: Poly(dimethylsiloxane), film thickness 3 m; carrier gas: He, 1,7 ml/min; EN 13628-1:2002 (E) 7 carrier gas split ratio: 1:20; injector temperature: 230 C; detector (flame ionization) temperature: 280 C; temperature programme: 50 C held for 5 min; raised to 100 C at 5 C/min raised to 250 C at 10
37、 C/min. NOTE 2A corresponding chromatogram for a mixture of solvents is shown in Figure 2. Key 1Methanol 2Ethanol 3Isopropanol 4Methylethyl ketone 5Ethyl acetate 6Isobutanol 7Isopropyl acetate 8n-propyl acetate 9Methylisobutyl ketone 10Ethoxypropanol 11Toluene 12n-butyl acetate 13Xylene 14Butyl cell
38、osolve ARetention time (min) BPeak height Figure 2 Example of chromatogram obtained with a capillary column EN 13628-1:2002 (E) 8 NOTE 3Other apparatus which is more specific to the alternative methods is identified under the relevant clauses. 6 Sampling Samples of packaging materials that are to be
39、 analysed shall be handled and stored so as to prevent either loss of volatile solvents or contamination by absorption of volatile solvents that may be present in the surrounding atmosphere. Sampling and analysis shall be done in a place where the air is solvent-free in order to reduce the problem o
40、f contamination of the samples from their surroundings due to the low concentrations of residual solvents in the samples. NOTESamples should be in tightly packed roll form if possible. Sheet samples can be prepared from the roll by cutting out a square window (several layers of sheets) with a knife.
41、 At least the first five layers should be discarded. When in the form of sheets they should be stacked tightly together to form a compact “block“ and wrapped tightly in a barrier material, preferably aluminium foil with a thickness of 30 m to 40 m. For storage periods of more than one hour the wrapp
42、ed samples should be stored at temperatures below 5 C and in an atmosphere free of volatile contaminants. 7 Test specimens 7.1 Specimen area in relation to vial volume The specimen area to be cut out shall depend on the vial volume and the level of residual solvents to be determined in the material.
43、 The ratio between the specimen area (in cm) and the vial volume (in ml) shall be between three and five. The specimens shall be cut out using an appropriate template (5.5). NOTEAs an example for a vial with a volume of 6 ml to 9 ml a specimen of 30 cm (2 cm 15 cm) can be used or proportional dimens
44、ions for other volumes. 7.2 Test specimens from sheets From the top of the sample take a block of about 15 to 20 sheets out without separating them. Immediately put back the remaining part of the sample in its packaging under the conditions specified in clause 6. Prepare a first vial; after withdraw
45、al of at least one layer (or more depending on the number of specimens to be prepared from the block) from the top of the block take the following sheet and rapidly cut the first specimen using a template (5.5). Coil the specimen rapidly and immediately put it into the vial. Crimp the vial immediate
46、ly to seal it. Prepare further specimens in the same way. The following precautions shall be taken. The different steps of the preparation shall be done very rapidly to avoid evaporation of the solvents. The sample sheet from which the specimen is cut shall be taken out of the block immediately befo
47、re preparation. The specimens shall always be cut at a defined place e.g. on the same drawing printed on the same place in the width and the template for cutting shall always be placed in the same manner. 8 Incubation of the test specimens 8.1 General Incubation time and temperature shall be optimiz
48、ed for each individual system in order to achieve a partition equilibrium of the residual solvents between the solid phase and the gas phase. With a certain temperature selected an optimum heating time shall be determined. EN 13628-1:2002 (E) 9 NOTE 1The time taken to reach partition equilibrium wil
49、l vary for different solvents depending on the boiling point and the absorptive properties of the materials to be analysed. NOTE 2As an initial guidance incubation, a temperature of 100 C for 60 min can be appropriate. However other incubation conditions depending on the materials and solvents to be analysed are also commonly used, e.g. temperature between 80 C and 150 C and heating times between 15 min and 60 min. Due to the sensitivity of the equilibrium to changes i
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