1、BS EN ISO21627-3:2009ICS 83.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Epoxyresins Determination ofchlorine contentPart 3: Total chlorine (ISO21627-3:2009)This British Standardwas published under theauthority of the StandardsPolicy and Strate
2、gyCommittee on 31 October2009 BSI 2009ISBN 978 0 580 62858 0Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21627-3:2009National forewordThis British Standard is the UK implementation of EN ISO21627-3:2009. It supersedes BS EN ISO 21627-3:2003 which iswithdrawn.The UK participat
3、ion 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 for its correct
4、application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21627-3 September 2009 ICS 83.080.10 Supersedes EN ISO 21627-3:2003English Version Plastics - Epoxy resins - Determination of chlorine content - Part 3
5、: Total chlorine (ISO 21627-3:2009) Plastiques - Rsines poxydes - Dtermination de la teneur en chlore - Partie 3: Chlore total (ISO 21627-3:2009) Kunststoffe - Epoxidharze - Bestimmung des Chlorgehaltes - Teil 3: Gesamtgehalt an Chlor (ISO 21627-3:2009) This European Standard was approved by CEN on
6、19 August 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 bibliographical references concerning such national standards may
7、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 member into its own language and notified to the CEN
8、 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, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherland
9、s, 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-1000 Brussels 2009 CEN All rights of exploitation in an
10、y form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21627-3:2009: EBS EN ISO 21627-3:2009EN ISO 21627-3:2009 (E) 3 Foreword This document (EN ISO 21627-3:2009) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN
11、/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 national standards shall be withdrawn at the latest by March
12、 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 EN ISO 21627-3:2003. According to the CEN/CENELEC Inte
13、rnal 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Ma
14、lta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21627-3:2009 has been approved by CEN as a EN ISO 21627-3:2009 without any modification. BS EN ISO 21627-3:2009ISO 21627-3:2009(E) ISO 2009 A
15、ll 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 results4 9 Precision 4 10 Test report5 Bibliography6 BS EN ISO 21627-3:2009ISO 21627-3:2009(E) iv ISO 200
16、9 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 technical committees. Each member body interested in a
17、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 closely with the International Electrotechnical Commission
18、 (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 International Standards adopted by the technical com
19、mittees 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 document may be the subject of patent rights. ISO shall not
20、 be held responsible for identifying any or all such patent rights. ISO 21627-3 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 21627-3:2002), which has been technically revised. ISO
21、 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 21627-3:2009ISO 21627-3:2009(E) ISO 2009 All rights reserved vIntroduction In prod
22、ucing 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 chemical activities differ significantly, so different ana
23、lytical 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 called ionic chlorine). Part 2: Easily saponifiable ch
24、lorine, 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 1-chloro-2-glycidylether (chloromethyl derivative) w
25、hich 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 impurities to be measured. For analytical methods for imp
26、urities 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 derivative) BS EN ISO 21627-3:2009BS EN ISO 21627-3:2009INTERN
27、ATIONAL STANDARD ISO 21627-3:2009(E) ISO 2009 All rights reserved 1Plastics Epoxy resins Determination of chlorine content Part 3: Total chlorine SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address
28、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 ISO 21627 specifies a method for the determination of the total amoun
29、t of chlorine in epoxy resins. The chlorine measured by this method, referred to as total chlorine, includes saponifiable organic chlorine and inorganic chlorine. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, o
30、nly the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods 3 Terms and definitions For the purposes of this document, the following terms an
31、d definitions apply. 3.1 total chlorine amount of chlorine measurable by this method NOTE It consists mainly of all saponifiable organic chlorine, e.g. 1,2-chlorohydrin, 1,3-chlorohydrin and 1-chloro-2-glycidylether which are the result of incomplete dehydrohalogenation, along with inorganic chlorin
32、e present in the test portion of epoxy resin. 4 Principle A test portion is dissolved in diethylene glycol monobutyl ether and the solution saponified with an alcoholic solution of potassium hydroxide by heating under reflux. The total chlorine content is then determined by potentiometric titration
33、of the solution with silver nitrate solution. BS EN ISO 21627-3:2009ISO 21627-3:2009(E) 2 ISO 2009 All rights reserved5 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water of grade 3 purity, as defined in ISO 3696:1987, or better. 5.1 Die
34、thylene glycol monobutyl ether. 5.2 Potassium hydroxide, 1 mol/l solution in 1,2-propanediol. Dissolve 56 g of potassium hydroxide in 1,2-propanediol, make up to 1 l with 1,2-propanediol and mix. 5.3 Glacial acetic acid. 5.4 Acetone. 5.5 Silver nitrate, 0,1 mol/l aqueous standard solution. 5.5.1 Pre
35、paration Dissolve 17 g of silver nitrate in water and make up to 1 l. 5.5.2 Standardization Weigh, to the nearest 0,1 mg, 5,845 g of sodium chloride previously dried at 500 C to 600 C, dissolve it in water and make up to 1 l to give a 0,1 mol/l solution. Pipette 5 ml of this solution into a 200 ml b
36、eaker and add 100 ml of acetone (5.4) and 2 ml of glacial acetic acid (5.3). Then titrate the solution potentiometrically with the silver nitrate solution prepared in 5.5.1. Carry out a blank test in the same way, but without the addition of sodium chloride. 5.5.3 Calculation of concentration Calcul
37、ate the concentration, to three significant figures, using the following equation: ()300,00558,5mcVV=where c3is 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 gram equivalent of
38、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). 5.5.4 Storage Store the silver nitrate solution in a brown bottle in the dark. 5.6 Si
39、lver nitrate, 0,01 mol/l aqueous standard solution. 5.6.1 Preparation Dissolve 1,7 g of silver nitrate in water and make up to 1 l. BS EN ISO 21627-3:2009ISO 21627-3:2009(E) ISO 2009 All rights reserved 35.6.2 Standardization Weigh, to the nearest 0,1 mg, 584 mg of sodium chloride previously dried a
40、t 500 C to 600 C, dissolve it in water and make up to 1 l to give a 0,01 mol/l solution. Pipette 5 ml of this solution into a beaker (6.10) and add 100 ml of acetone (5.4) and 2 ml of glacial acetic acid (5.3). Then titrate the solution potentiometrically with the silver nitrate solution prepared in
41、 5.6.1. Carry out a blank test in the same manner, omitting the sodium chloride. 5.6.3 Calculation of concentration Calculate the concentration from the equation in 5.5.3, rounding the result to three significant figures. 5.6.4 Storage Store the silver nitrate solution in a brown bottle in the dark.
42、 6 Apparatus Usual laboratory apparatus, plus the following: 6.1 Potentiometric-titration apparatus, comprising a suitable potentiometer equipped with a silver electrode and a silver chloride or mercury sulfate electrode and a titration stand. 6.2 Analytical balance, accurate to 0,1 mg. 6.3 Volumetr
43、ic flask, of capacity 1 l. 6.4 Hotplate or oil bath, capable of being heated to above 200 C. 6.5 Conical flask, of capacity 200 ml, with a ground-glass stopper. 6.6 Reflux condenser. 6.7 Graduated glass cylinder, of capacity 50 ml. 6.8 Pipette, of capacity 5 ml. 6.9 Porcelain crucible. 6.10 Beaker,
44、of capacity 200 ml. 6.11 Magnetic stirrer, with a PTFE (polytetrafluoroethylene) coated stirring bar. 7 Procedure 7.1 Into a 200 ml conical flask (6.5), weigh, to the nearest 0,1 mg, a test portion of a size such that it contains 0,5 mg to 1,5 mg of chlorine when the expected total chlorine content
45、is less than 1 % or a test portion of a size such that it contains 5 mg to 15 mg of chlorine when the expected total chlorine content is greater than 1 %. 7.2 Add 25 ml of diethylene glycol monobutyl ether (5.1) and dissolve the test portion using a magnetic stirrer (6.11). 7.3 Add 25 ml of potassiu
46、m hydroxide solution in 1,2-propanediol (5.2). Reflux the solution on a hotplate or in an oil bath (6.4) for 10 min while stirring. BS EN ISO 21627-3:2009ISO 21627-3:2009(E) 4 ISO 2009 All rights reserved7.4 Leave to cool, then pour 5 ml of acetone (5.4) down the reflux condenser. 7.5 Transfer the s
47、olution from the flask to a 200 ml beaker (6.10). Wash the inside of the flask three times with glacial acetic acid (5.3), using a total of 50 ml of acid and adding the washings to the solution in the beaker. 7.6 Immerse the electrodes (see 6.1) in the solution. Adjust the stirrer speed to give vigo
48、rous stirring without splashing. 7.7 Carry out the potentiometric titration with 0,01 mol/l silver nitrate solution (5.6) if the expected total chlorine content is less than 1 % or with 0,1 mol/l silver nitrate solution (5.5) if the expected total chlorine content is greater than 1 %. 7.8 Carry out
49、a blank test in the same way. 8 Expression of results Calculate the total chlorine content, using the following equation: ()3123035,5 1000(Cl )cVVwm = where w3(Cl) is the total chlorine content of the sample, expressed in milligrams per kilogram (mg/kg); V1is the volume of silver nitrate solution (5.5 or 5.6) used in the titration of the test portion, expressed in millilitres (ml); V2is the volume of silver nitrate solution used in the blank test, expressed in millilitres (ml); c3is the concentration of the si
