1、BRITISH STANDARD BS EN 13628-22002 Packaging - Flexible packaging material - Determination of residual solvents by static headspace gas chromatography - Part 2: Industrial methods The European Standard EN 13628-2:2002 has the status of a British Standard ICs 55.040 NO COPYING WITHOUT BSI PERMISSION
2、EXCEPT AS PERMITTED BY COPYRIGHT LAW - British Standards BS EN 13628-2:2002 Amd. No. Date ISBN O 580 40626 1 National foreword Comments This British Standard is the official English language version of The UK participation in its preparation was entrusted by Technical Committee PKW/5, Primary and tr
3、ansport packaging, to Subcommittee PKW/5/26, Packaging made from flexible materials, which has the responsibility to: EN 13628-212002. - - aid enquirers to understand the text; present to the responsible internationaYEuropean committee any enquiries on the interpretation, or proposals for change, an
4、d keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. - A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or Eur
5、opean publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include
6、all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. This British Standard, having been prepared under the direction of the Consumer Products and services Sector an
7、d Strategy was published under the authority of the Standards Policy and Strategy Committee on 21 October 2002 Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright date displayed in t
8、his document indicates when the was last issued. Amendments issued since publication O BSI 21 October 2002 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13628-2 October 2002 ICs 55.040 English version Packaging - Flexible packaging material - Determination of residual solvents by static heads
9、pace gas chromatography - Part 2: Industrial methods Emballage - Matriaux demballages souples - Dtermination des solvants rsiduels par chromatographie en phase gazeuse et espace de tte statique - Partie 2: Mthodes industrielles Verpackung - Flexible Packstoffe - Bestimmung der Restlsemittel durch st
10、atische Dampfraumanalyse mittels Gaschromatographie - Teil 2: Industrielle Verfahren This European Standard was approved by CEN on 26 August 2002. CEN members are bound to comply with the CENICENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of
11、a national standard without any alteration. Up-to-date lists and bibliographical references 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 i
12、n any other language made by translation under the responsibility of a CEN member into its 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, Ger
13、many, Greece, Iceland. Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMIITEE FOR STANDARDIZATION EUROPISCHES KOMITEE FR NORMUNG COMIT EUROPEN DE NORMALISATION Management Centre: rue de Stassart, 36 8-1050 Brussels O 2002 C
14、EN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13628-2:2002 E EN 13628-22002 (E) Contents Page Foreword 3 1 2 3 4 5 6 7 8 9 10 11 Scope 4 Normative references 4 Principle 4 Reagents . 5 Apparatus . 5 Sampling . 8 Test specimens 8 I
15、ncubation of the test specimens . 8 Procedure . 9 Precision data . 12 Test report 12 2 EN 33628-2:2002 (E) Foreword This document EN 13628-2:2002 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 stat
16、us of a national standard, either by publication of an identical text or by endorsement, at the latest by April 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
17、chromatography, which is published in two parts: - Part I: Absolute methods - Part 2: Industrial methods This part of EN 13628 should be read in conjunction with EN 13628-1. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to
18、 implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. 3 EN 13628-2:2002 (E) 1 Scope This part of this European Stand
19、ard specifies rapid methods as commonly used in quality control for monitoring the level of residual solvents used in the production of flexible packaging by static headspace chromatography. The procedures described in this part involve one single injection of the headspace which implies an incomple
20、te extraction of the solvent. The values obtained may be lower than the absolute content which should be determined according to Part 1. Residues from thermal decomposition products are not within the scope of this standard. The method is applicable to flexible packaging materials that may consist o
21、f mono- or multilayer plastic films, paper or board, foil or combinations thereof. This method does not apply to residual solvents with amounts lower than 0,5 mglm?. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These no
22、rmative references are cited at the appropriate places in the text, and 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 r
23、eferences the latest edition of the publication referred to applies (including amendments). IS0 2859-1, Sampling procedures for inspection by attributes - Part I: Sampling schemes indexed by acceptance quality limit (AQL) for lot-by-lot inspection. IS0 2859-2, Sampling procedures for inspection by a
24、ttributes - Part 2: Sampling plans indexed by limiting quality (LQ) for isolated lot inspection. IS0 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 Prin
25、cipie Specimens of the flexible packaging material are placed in a hermetically 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 th
26、e headspace into a gas chromatograph for analysis. The transfer may be performed: a) by specific semi-automatic or automatic systems which allow pressurization of the heated vials; b) manually or automatically by using a heated gastight syringe or a loop without pressurization of the heated vials. T
27、he relative amount of residual solvent is determined by single headspace extraction using external or internal standards. NOTE For reproducibility the same incubation conditions should be used for each single analysis. During the analysis, there could be interferences from possible products of therm
28、al decomposition. Additional peaks due to these products should not be considered for evaluation of residual solvents. 4 EN 73628-22002 (E) 4 Reagents 4.1 General All reagents shall be of a recognized analytical reagent grade. NOTE Grades stated as being suitable for chromatography car; be commercia
29、lly available and are recommended for use as reference for standard calibration solutions. Appropiate safety precautions should be used when handling toxic and/or flammable solvents. 4.2 Reference solvents, for the preparation of standard calibration solutions. 4.3 Dilution solvent, with a retention
30、 time different from those of residual solvents in the sample. NOTE Solvents such as hexane, cyclohexanaone, acid amides 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 access
31、ory equipment, for example, the headspace sampler, fitted with an inert septum seal and aluminium crimp tops. The septum 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 subseq
32、uent analysis. NOTE Elastomers lined with polytetrafluoroethylene (PTFE) are suitable materials for septum seals. 5.2 Crimping 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,l mg. 5.5 Template, for cutti
33、ng samples. The dimensions of this template shall be matched to the vial volume used. 5.6 Scalpel, or sharp knife. 5.7 Syringes (e.g. 1 pl, 10 pl) 5.8 Gas chromatograph, having a flame ionization detector or equivalent for the solvents to be determined. 5.9 Gas chromatographic column, either packed
34、or capillary, that will give good resolution of the solvents to be determined from any other components that might be injected 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: 80/1
35、20 mesh graphitised carbon, deactivated with polyethyleneglycol; carrier gas: NZi 20 ml/min; injector temperature: 220 OC; temperature programme: 80 OC; raised to 160 OC at 6 OC/min; raised to 225 OC at I ,5 “C/min; held for 16 min 5 EN 13628-22002 (E) NOTE 1 A correspondincj chromatogram obtained f
36、or a mixture of solvents is shown in Figure 1 2 1 b 4 9. A Key 1 4,23 methanol 2 6,67 ethanol 3 925 acetone 4 17, 06 ethyl acetate 5 19,l butanol 6 23,34 trichloroethylene 7 28,4 isobutyl acetate 8 33,87 methyl isobutyl ketone 9 41,86 toluene 10 64.06 xylene A Retention time (min) B Peak height Figu
37、re 1 - Example of chromatogram obtained with a packed column or b) Capillary column: (fused silica): length : 30 m; internal diameter : 0,32 mm; stationary phase : Poly(dimethylsiloxane) film thickness 3pm; carrier gas : He I ,7ml/min; carrier gas split ratio : 1 :20; injector temperature : 230 OC;
38、detector (flame ionisation) temperature : 280 OC; 6 EN q3628-2:2002 (E) L temperature programme: 50 OC held for 5 min; raised to 1 O0 OC ai 5 “Clmin: raised to 250 OC at IC! “Clmin. NOTE 2 A correspondin chromatogram is shown in Figure 2. B 1 1 2 2.5 Key 1 Methanol 2 Ethanol 3 IsoDroDanol 3 0,5 7 6
39、a 7 I 10 12,5 A 9 11 3 L 12 -r 13 14 17,5 20 4 5 6 7 8 9 10 11 12 13 14 Meihyi ethyl ketone Ethyl acetate Isobutanol Isopropyl acetate n-propyl acetate Methyl isobutyl ketone Etoxypropanol Toluene n-butyl acetate Xylene Butyl cellosolve A Retention time (min) B Peak height Figure 2 - Example of chro
40、matogram obtained with a capillary column NOTE Other apparatus which is more specific to the alternative methods is identified under the relevant clauses. 7 EN 13628-22002 (E) 6 Sampling Sampling shall be in accordance with interna! quality control procedures Sampling shall follow IS0 2859-1 and IS0
41、 2859-2. Samples of packaging materials that are to be analyzed 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 th
42、e air is solvent-free to reduce the problem of contamination from the surroundings due to the low concentration of residual solvents in the samples. NOTE If samples need to be stored they should be in tightly packed roll form if possible. Sheet samples may be prepared from the roll by cutting out a
43、square window (several layers of sheets) with a knife. When in 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 p to 40 pm. For storage periods of more than one hour the wrapped
44、 samples should be stored at temperatures below 5 OC 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.
45、Usually the ratio between the specimen area (in cm) and the vial volume (in mi) shall be between three and five. The specimens shall be cut out using.an appropriate template (5.5). NOTE proportional dimensions for other volumes. As an example, for a vial with a volume of 6 ml to 9 ml a specimen of 3
46、0 cmz (2 cm x 15 cm) can be used or 7.2 Test specimens From a representative sample (see clause 6) cut a specimen using a template (5.5). Coil the specimen rapidly and immediately put it into the vial. Crimp the vial immediately to seal it. The following precautions shall be taken: - the different s
47、teps of the preparation shall be done very rapidly to avoid evaporation of the solvents; -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 t
48、est specimens Incubation temperature and time shall be chosen to suit the materials being tested and the solvents likely to be present. Conditions used shall be included in the test report. NOTE Incubation conditions of 110 OC for 20 min are recommended. In order to compare residual solvent levels,
49、incubation conditions used shall be the same. To ensure repeatability, the temperature shall be accurate to ?- 2 OC and time shall be accurate to k 0,5 min. 8 EN 13628-22002 (E) 9 Procedure 9.1 General Quantitative analysis of residual solvents shall be carried out using one of the two methods of static headspace chromatography described in this clause, as appropriate. The methods are: - semi-automatic or automatic injection (see 9.2); and - manual injection (see 9.3). 9.2 Semi-automatic or automatic injection 9.2.1 General This method shall be used where a semi-automatic
