1、BS EN ISO21627-2:2009ICS 83.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Epoxyresins Determination ofchlorine contentPart 2: Easily saponifiable chlorine(ISO 21627-2:2009)This British Standardwas published under theauthority of the StandardsPol
2、icy and StrategyCommittee on 31 October2009 BSI 2009ISBN 978 0 580 62857 3Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21627-2:2009National forewordThis British Standard is the UK implementation of EN ISO21627-2:2009. It supersedes BS EN ISO 21627-2:2003 which iswithdrawn.The
3、 UK participation in its preparation was entrusted to TechnicalCommittee PRI/52, Adhesives.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 fo
4、r its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21627-2 September 2009 ICS 83.080.10 Supersedes EN ISO 21627-2:2003English Version Plastics - Epoxy resins - Determination of chlorine co
5、ntent - Part 2: Easily saponifiable chlorine (ISO 21627-2:2009) Plastiques - Rsines poxydes - Dtermination de la teneur en chlore - Partie 2: Chlore facilement saponifiable (ISO 21627-2:2009) Kunststoffe - Epoxidharze - Bestimmung des Chlorgehaltes - Teil 2: Leicht verseifbares Chlor (ISO 21627-2:20
6、09) This European Standard was approved by CEN on 18 September 2009. 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 bibliographic
7、al references concerning such national standards 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 translation under the responsibility of a CEN
8、 member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, It
9、aly, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-10
10、00 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21627-2:2009: EBS EN ISO 21627-2:2009EN ISO 21627-2:2009 (E) 3 Foreword This document (EN ISO 21627-2:2009) has been prepared by Technical Committee ISO/TC 61 “Pl
11、astics“ 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 2010, and conflicting nationa
12、l standards shall be withdrawn at the latest by March 2010. 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 document supersedes E
13、N ISO 21627-2:2003. 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, Greece, Hungary, Icela
14、nd, 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 21627-2:2009 has been approved by CEN as a EN ISO 21627-2:2009 without any modification.
15、 BS EN ISO 21627-2:2009ISO 21627-2:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Principle .1 5 Reagents 2 6 Apparatus.3 7 Procedure.3 8 Expression of results5 9 Precision 5 10 Test report5 Bibliography6
16、 BS EN ISO 21627-2:2009ISO 21627-2:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO te
17、chnical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates close
18、ly with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted 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
19、 International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard 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 docume
20、nt may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 21627-2 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 2
21、1627-2:2002), which has been technically revised. ISO 21627 consists of the following parts, under the general title Plastics Epoxy resins Determination of chlorine content: Part 1: Inorganic chlorine Part 2: Easily saponifiable chlorine Part 3: Total chlorine BS EN ISO 21627-2:2009ISO 21627-2:2009(
22、E) ISO 2009 All rights reserved vIntroduction In producing epoxy resins based on epichlorohydrin, impurities containing chlorine may be formed. These are shown below. Since these impurities could impair the final properties of the cured resins, it is necessary to control their formation. Their chemi
23、cal activities differ significantly, so different analytical procedures are needed for their analysis. ISO 21627 specifies methods for the determination of these organic and inorganic chlorides which occur as impurities in epoxy resins derived from epichlorohydrin: Part 1: Inorganic chlorine (also c
24、alled ionic chlorine). Part 2: Easily saponifiable chlorine, consisting mainly of chlorine which is present as 1,2-chlorohydrin as the result of incomplete dehydrohalogenation. Part 3: Total chlorine, consisting mainly of all saponifiable organic chlorine, e.g. 1,2-chlorohydrin, 1,3-chlorohydrin and
25、 1-chloro-2-glycidylether (chloromethyl derivative) which are the result of incomplete dehydrohalogenation, along with inorganic chlorine present in the test portion of epoxy resin. Since the purposes of Parts 1 to 3 of ISO 21627 differ, one of these methods should be selected, depending on the impu
26、rities to be measured. For analytical methods for impurities other than those shown below, see ISO 4615. Typical types of inorganic and organic chlorine impurity are shown below: Inorganic chlorine (or ionic chlorine) 1,2-Chlorohydrin 1,3-Chlorohydrin 1-Chloro-2-glycidylether (chloromethyl derivativ
27、e) BS EN ISO 21627-2:2009BS EN ISO 21627-2:2009INTERNATIONAL STANDARD ISO 21627-2:2009(E) ISO 2009 All rights reserved 1Plastics Epoxy resins Determination of chlorine content Part 2: Easily saponifiable chlorine SAFETY STATEMENT Persons using this document should be familiar with normal laboratory
28、practice, if applicable. This document does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope This part of IS
29、O 21627 specifies a method for the determination of easily saponifiable chlorine in epoxy resins. The easily saponifiable chlorine content is the quantity of easily saponifiable chlorine in a given quantity of epoxy resin. The values obtained are indicative of the concentration of easily saponifiabl
30、e chlorine in chlorohydrin groups in the resin. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any
31、 amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 21627-1, Plastics Epoxy resins Determination of chlorine content Part 1: Inorganic chlorine 3 Terms and definitions For the purposes of this document, the following terms and definitions apply
32、. 3.1 easily saponifiable chlorine amount of chlorine saponifiable by this test method, consisting mainly of chlorine present as 1,2-chlorohydrin as a result of incomplete dehydrohalogenation 4 Principle Epoxy resins, except glycidyl esters, are reacted with NaOH solution at room temperature in 2-bu
33、toxyethanol. Glycidyl esters are reacted with NaOH solution at 50 C in methanol. BS EN ISO 21627-2:2009ISO 21627-2:2009(E) 2 ISO 2009 All rights reservedThe mixture is acidified and the concentration of chloride ions resulting from the saponification is determined by potentiometric titration with st
34、andardized silver nitrate solution. A correction is made for the inorganic chlorine content of the sample, determined by the method specified in ISO 21627-1. 5 Reagents During the analysis, use only reagents of recognized analytical grade and water of grade 3 purity, as defined in ISO 3696:1987, or
35、better. 5.1 Glacial acetic acid. 5.2 2-Butoxyethanol (ethylene glycol monobutyl ether), stored in a brown bottle in the dark. WARNING 2-Butoxyethanol is toxic. Avoid inhalation of vapour. Prevent contact with skin and eyes. Work under a fume hood or in a well-ventilated area. The threshold limit val
36、ue is a volume fraction of 5 105. 5.3 2-Butanone (methyl ethyl ketone). 5.4 Methanol. WARNING Methanol is toxic. Avoid inhalation of vapour. Prevent contact with skin and eyes. Work under a fume hood or in a well-ventilated area. 5.5 Sodium hydroxide, 120 g/l solution in 2-butoxyethanol (for epoxy r
37、esins); in methanol (for glycidyl esters). Dissolve 120 g of sodium hydroxide in 75 ml of water plus sufficient 2-butoxyethanol (5.2) or methanol (5.4) to achieve complete dissolution. Cool and make up to 1 l with the same solvent. 5.6 Acetone. 5.7 Silver nitrate solution, 0,01 mol/l. 5.7.1 Preparat
38、ion Dissolve 1,7 g of silver nitrate in water and make up to 1 l. 5.7.2 Standardization Weigh, to the nearest 0,1 mg, 584 mg of sodium chloride, previously dried at 500 C to 600 C, and dissolve in 1 l of water. Pipette 5 ml of this solution into a 200 ml beaker and add 100 ml of acetone (5.6) and 2
39、ml of glacial acetic acid (5.1). Then titrate potentiometrically with the silver nitrate solution prepared in 5.7.1. Conduct a blank test in the same way, leaving out the sodium chloride. BS EN ISO 21627-2:2009ISO 21627-2:2009(E) ISO 2009 All rights reserved 35.7.3 Calculation of concentration Calcu
40、late the concentration using the following equation, rounding the result to three significant figures: ()200,00558,5mcVV=where c2is the concentration of the silver nitrate solution, expressed in moles per litre (mol/l); m is the mass of sodium chloride used, expressed in milligrams (mg); 58,5 is the
41、 gram equivalent of sodium chloride (g/mol); V is the volume of silver nitrate solution used in the titration, expressed in millilitres (ml); V0is the volume of silver nitrate solution used in the blank, expressed in millilitres (ml). 5.7.4 Storage Store the silver nitrate solution in a brown bottle
42、 in the dark. 6 Apparatus Usual laboratory apparatus, plus the following: 6.1 Potentiometric-titration apparatus, comprising a suitable potentiometer or autotitrator equipped with a glass-silver/silver chloride electrode system, titration stand and 10 ml microburette. 6.2 Analytical balance, accurat
43、e to 0,1 mg. 6.3 Beaker, of capacity 200 ml. 6.4 Volumetric flask, of capacity 1 l. 6.5 Pipettes, of capacities 2 ml, 5 ml and 25 ml. 6.6 Graduated glass cylinder, of capacity 100 ml. 6.7 Water bath, capable of being maintained at 50 C. 6.8 Conical flask, of capacity 200 ml, with a ground-glass stop
44、per. 6.9 Reflux condenser. 6.10 Magnetic stirrer, with a PTFE (polytetrafluoroethylene) coated stirring bar. 7 Procedure 7.1 Epoxy resins 7.1.1 Weigh, to the nearest 0,1 mg, a test portion containing not more than 1,78 mg of easily saponifiable chlorine into the beaker (6.3). Pipette 25 ml of 2-buto
45、xyethanol (5.2) into the beaker and dissolve the test portion using the magnetic stirrer (6.10) and by heating, if necessary. Cool the solution to room temperature BS EN ISO 21627-2:2009ISO 21627-2:2009(E) 4 ISO 2009 All rights reservedand pipette 25 ml of sodium hydroxide solution in 2-butoxyethano
46、l (see 5.5) into the beaker. Mix well, cover the beaker and allow the reaction mixture to stand at room temperature for 2 h. 7.1.2 For quality-control purposes, a shorter saponification time of 30 min is permissible if it can be shown to give similar results. This shall be recorded in the test repor
47、t. 7.1.3 Add 100 ml of 2-butanone (5.3) and 25 ml of acetic acid (5.1) to the mixture while stirring. Stir for a few minutes more until all of the precipitate which is formed during the addition of the acetic acid has dissolved. 7.1.4 Place the electrodes (see 6.1) in the test solution and titrate t
48、he solution potentiometrically with silver nitrate solution (5.7). It is essential to carry out the titration as soon as possible after adding the acetic acid, otherwise lower values might be obtained. 7.1.5 Carry out a blank test at the same time as the determination, following the same procedure a
49、nd using the same reagents but omitting the test portion. If it is found that less than 1 ml of silver nitrate solution is required for the titration (and thus also for the blank titration), repeat the test with exactly 1 ml, accurately measured, of 0,01 mol/l potassium chloride solution added to the solution (and also to the blank test solution) prior to the titration. Titrate immediately after addition of the potassium chloride solution. 7.1.6 Determine the inorganic chlorine content of the sample i
