1、BRITISH STANDARD Adhesives - Determination of free monomer content in adhesives based on synthetic polymers O The European Standard EN 12963:2001 has the status of a British Standard ICs 83.180 BS EN 12963:2001 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN 12963:2001 T
2、his British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 June 2001 O BSI 06-2001 ISBN O 580 37432 7 National foreword This British Standard is the offic
3、ial English language version of EN 12963:2001. The UK participation in its preparation was entrusted to Technical Committee PRU52, Adhesives, which has the responsibility to: - - aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation,
4、or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. - A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implem
5、ent international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purpor
6、t to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. o o a Summary of pages This document comprises a front cover, an inside fro
7、nt cover, the EN title page, pages 2 to 7 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. fiate Comments EUROPEAN STANDARD 0 NORME EUROPENNE EUROPISCHE NORM EN 12963 April 2001 English versi
8、on Adhesives - Determination of free monomer content in adhesives based on synthetic polymers Adhsifs - Dtermination de la teneur en monomres libres dans des adhsifs base de polymres synthtiques Klebstoffe - Bestimmung des freien Monomeranteils in Klebstoffen auf der Basis synthetischer Polymere Thi
9、s European Standard was approved by CEN on 1 March 2001. CEN members are bound to comply with the CENKENELEC 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
10、 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 its
11、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, Netherlands, Norway, Portugal, Spain, Sw
12、eden, Switzerland and United Kingdom. EUROPEAN COMMI1TEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels O 2001 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national M
13、embers. Ref. No. EN 12963:2001 E Page 2 EN 12963:2001 Contents . Page Foreword 3 1 2 3 4 5 6 7 8 9 10 11 12 13 Scope 4 Normative references 4 Terms and definitions . 4 Principle 4 Safety 4 Chemicals . 4 Apparatus . 5 Sampling and sample preparation . 5 Chromatographic conditions . 5 Calibration of t
14、he gas chromatograph 6 Procedure . 6 Expression of results 7 Test report 7 Page 3 EN 12963:2001 Foreword This European Standard has been prepared by Technical Committee CENTTC 193 “Adhesives“, the secretariat of which is held by AENOR. This European Standard shall be given the status of a national s
15、tandard, either by publication of an identical text or by endorsement, at the latest by October 2001, and conflicting national standards shall be withdrawn at the latest by October 2001. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries
16、 are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Page 4 EN 12963:2001 1 Scope O This European Standard sp
17、ecifies a simple test method for the gas-chromatographic determination of free monomer content in polymeric adhesives after specific treatment. This test method can be used for the determination of acrylic, styrene, vinyl and other unsaturated monomers. NOTE This method could also be used for the de
18、termination of other monomers, if applicable. 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 and the publications are listed hereafter. For dated
19、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 (including amendments). EN 923 Adhesives -Terms and d
20、efinitions EN 1066 Adhesives - Sampling EN 1067 Adhesives - Examination and preparation of samples for testing 3 Terms and definitions For the purposes of this European Standard, the terms and definitions given in EN 923 apply. 4 Principle 4.1 Water-borne adhesives An aliquot of an extract of the wa
21、ter-borne adhesive to be analysed is injected into a gas chromatograph equipped with a capillary column and a linear temperature programmer. The monomers are detected by a Flame Ionisation Detector (FID). Quantification is made by peak area measurement. O 4.2 Solvent-borne or solvent-less adhesives
22、An aliquot of the solvent-borne or solventless adhesive is diluted with a suitable solvent. The solvent shall be able to considerably reduce the viscosity of the adhesive solution as to allow it to be injected into the gas chromatrograph. The solvent shall not interfere with the monomers to be detec
23、ted. The diluted solution is analysed as the extract as described in 4.1 5 Safety Persons using this standard shall be familiar with normal laboratory practice. This standard does not purport to address all the safety problems, if any, associated with its use. It is the responsibility of the user to
24、 establish safety and health practices and to ensure compliance with any European or national regulatory conditions. 6 Chemicals All the chemicals used for the test shall be of analytical grade. Page 5 EN 12963:2001 07 Apparatus Ordinary laboratory apparatus and, 7.1 Analytical balance, accurate to
25、Oll mg. 7.2 Ultrasonic bath. 7.3 Vials, of a 6 ml capacity. 7.4 Gas chromatograph, having a FID detector and a linear temperature programmer. 7.5 Capillary column, of 30 m length, 0,32 mm internal diameter, and silica coated with a film of polyethyleneglycol 20 M of 1 pm thickness. Other columns hav
26、ing equivalent or superior performances may also be used. 7.6 Integrator or suitable recorder The recorder shall have a full scale deflection of 10 mV, a full scale response time of 2 s or less, and a maximum noise level of f 0,03%. 7.7 Microsyringe, of a 10 pl to 50 pl capacity graduated to 1 pi. 8
27、 Sampling and sample preparation A sample of the adhesive shall be taken in accordance with EN 1066 and prepared for testing in accordance with EN 1067. 9 Chromatographic conditions Typical operating conditions (may be modified according to separation problems, if noted in the test report). Carrier
28、: Hydrogen Column flow: 1,5 ml/min Split flow : 5 ml/min Carrier pressure : 20 kPa Injector temperature : 350 “C Detector temperature : 350 OC Initial temperature : 50 OC Initial time : 5 min Rate : 30 “C/min Final temperature : 190 OC Total analysis time : 16,5 min Page 6 EN 12963:2001 10 Calibrati
29、on of the gas chromatograph a 10.1 External standard method Determine the response areas and the retention times of each monomer expected to be present in the adhesive by injecting samples of a standard amount of 4 pI with various concentrations of each monomer. Measure the peak areas of the individ
30、ual components and plot the areas versus their amounts. 10.2 Internal standard method Determine the response factors and the retention times of each component expected to be present in the adhesive by injecting a solution containing measured amounts of an internal standard and of the single componen
31、t. The solvent shall be the same as the one used for the sample analysis (1 1). Calculate the peak areas and calculate the relative response factor, RF, using the following equation: As x Wc RF= AcxWs a where : As = peak area of the internal standard Ac= peak area of the single component Ws =weight
32、of the internal standard Wc =weight of the single component 11 Procedure 11.1 General If the internal standard method is chosen (10.2), prepare the internal standard solution measuring a proper amount of internal standard and dissolving it in the solvent to be used for the extraction (1 1.2) or for
33、the dilution (1 1.3 and e 11.4). In the case 1 1.2 the internal standard should be preferably soluble in the extraction solvent in order to separate it quantitatively from the water phase. Inject 4 pl of solvent phase. The volume has to be precise if the external standard method is used. 11.2 Water-
34、borne adhesives For water-borne adhesives weight in a vial (7.3) 3 g of adhesive using the balance (7.1), add exactly 5 ml of hexane and plug the vial. Put the vial in the ultrasonic bath (7.2) for 10 min to promote the extraction. Remove the vial from the bath, allow to settle for 15 min. The two p
35、hases will separate clearly. Other solvents can be used instead of hexane. They shall be able to extract quantitatively the monomers and clearly separate from water. 11.3 Solvent-borne adhesives For solvent-borne adhesives weight 1 g of solution. If necessary, dilute with solvent to obtain an inject
36、able solution. a For diluting, one of the solvents already contained in the solvent-borne adhesive, is to be preferred. Page 7 EN 12963:2001 Plug the vial and stir to homogenise. 11.4 Solventless adhesives For solventless adhesives make a solution in a suitable solvent and proceed as described in 11
37、.2. The solvent shall not interfere with the monomers to be analyzed. 12 Expression of results Determine the concentration of each component as appropriate : a) if the external standard method is followed, calculate the concentration of the component dividing the absolute amount obtained in the cali
38、bration curve (in pg) by the weight of the samples (in grammes) ; b) if the internal standard method is followed, calculate the concentration using the ecuation given below Ac x RF x Cs x Ws C= As x Wd Where C = concentration of the single component in milligrammes per kilogram Ac = peak area of the
39、 same component RF = relative response factor of the same component Cs = concentration of the internal standard in the internal standard solution in milligrammes per kilogram Ws = weight of the internal standard solution in grammes As = peak area of the internal standard Wd = weight of the original
40、sample in grammes 13 Test report The test report shall include : a) reference to this European Standard ; b) the type and designation of the adhesive tested ; c) the result of the test expressed in accordance with clause 12 ; d) any modification to the procedure described and any circumstances which
41、 may have affected the result (sample preparation, extraction solvent, calibration, etc.) ; e) the date of the test. BS EN 12963:2001 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution 3SI is the independent national body responsible for preparing 3ritish Standards. It pres
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