1、January 2010DEUTSCHE NORM English price group 8No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 83.080.10!$V“1565192www
2、.din.deDDIN EN ISO 21627-2Plastics Epoxy resins - Determination of chlorine content Part 2: Easily saponifiable chlorine (ISO 21627-2:2009)English version of DIN EN ISO 21627-2:2010-01Kunststoffe Epoxidharze - Bestimmung des Chlorgehaltes Teil 2: Leicht verseifbares Chlor (ISO 21627-2:2009)Englische
3、 Fassung DIN EN ISO 21627-2:2010-01SupersedesDIN EN ISO 21627-2:2004-05www.beuth.deDocument comprises pages12DIN EN ISO 21627-2:2010-01 National foreword This standard has been prepared by Technical Committee ISO/TC 61 “Plastics” (Secretariat: ANSI, USA) in collaboration with Technical Committee CEN
4、/TC 249 “Plastics”, (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-02-01 AA Hrtbare Harze. The DIN Standards corresponding to the International Standards referred to in
5、this document are as follows: ISO 3696 DIN ISO 3696 ISO 21627-1 DIN EN ISO 21627-1 Amendments This standard differs from DIN EN ISO 21627-2:2004-05 as follows: a) In clause 5 “Reagents”, “Sodium chloride” (5.6) has been deleted and subsequent subclauses have been renumbered. b) Under “Silver nitrate
6、 solution, 0,01 mol/l” (5.7), the equation in subclause 5.7.3 (formerly 5.8.3) “Calculation of concentration” has been modified in that the gram equivalent of sodium chloride (g/mol) is 58,5 (instead of 58,45). c) In subclauses 5.7.3 (formerly 5.8.3) “Calculation of concentration” and 8 “Expression
7、of results”, the gram equivalent of sodium chloride and of chlorine respectively is given. d) In clause 6 “Apparatus”, the specifications relating to the potentiometric-titration apparatus (6.1) have been rendered more precise. e) In clause 6 “Apparatus”, “Conical flask” (6.8), “Reflux condenser” (6
8、.9) and “Magnetic stirrer” (6.10) have been added. f) Subclause 7.2 “Glycidyl esters” of clause 7 “Procedure” has been completely revised. g) The standard has been editorially revised. Previous editions DIN 54812: 1987-12 DIN EN ISO 4583: 1998-06 DIN EN ISO 21627-2: 2004-05 National Annex NA (inform
9、ative) Bibliography DIN EN ISO 21627-1, Plastics Epoxy resins Determination of chlorine content Part 1: Inorganic chlorine DIN ISO 3696, Water for analytical laboratory use Specification and test methods 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21627-2 September 2009 ICS 83.080.10
10、Supersedes EN ISO 21627-2:2003English Version Plastics - Epoxy resins - Determination of chlorine content - 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) Kunststo
11、ffe - Epoxidharze - Bestimmung des Chlorgehaltes -Teil 2: Leicht verseifbares Chlor (ISO 21627-2:2009) 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 St
12、andard the status of a national standard without any alteration. Up-to-date lists and bibliographical 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, Fre
13、nch, 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus
14、, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMI
15、T EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 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: EContents Page Foreword .3 Introduction.4 1 Scope
16、5 2 Normative references5 3 Terms and definitions .5 4 Principle .5 5 Reagents 6 6 Apparatus.7 7 Procedure.7 8 Expression of results9 9 Precision 9 10 Test report9 Bibliography10 EN ISO 21627-2:2009 (E) DIN EN ISO 21627-2:2010-01 2Foreword This document (EN ISO 21627-2:2009) has been prepared by Tec
17、hnical Committee ISO/TC 61 “Plastics“ 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
18、 2010, and conflicting national 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 righ
19、ts. This document supersedes EN 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, G
20、ermany, Greece, Hungary, Iceland, 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:
21、2009 without any modification. EN ISO 21627-2:2009 (E) DIN EN ISO 21627-2:2010-01 3Introduction 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
22、 necessary to control their formation. Their chemical 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 e
23、pichlorohydrin: Part 1: Inorganic chlorine (also called 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 chl
24、orine, e.g. 1,2-chlorohydrin, 1,3-chlorohydrin and 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
25、 methods should be selected, depending on the impurities 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-Chlorohydri
26、n 1-Chloro-2-glycidylether (chloromethyl derivative) EN ISO 21627-2:2009 (E) DIN EN ISO 21627-2:2010-01 4SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address all of the safety concerns, if any, assoc
27、iated 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 easily saponifiable chlorine in epoxy resins. The easily
28、 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 saponifiable chlorine in chlorohydrin groups in the resin. 2 Normative references The following referenced documents ar
29、e 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 amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO
30、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. 3.1 easily saponifiable chlorine amount of chlorine saponifiable by this test method, consisting mainly of
31、 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-butoxyethanol. Glycidyl esters are reacted with NaOH solution at 50 C in methanol. EN ISO 21627-2:2009 (E) DIN
32、 EN ISO 21627-2:2010-01 5The mixture is acidified and the concentration of chloride ions resulting from the saponification is determined by potentiometric titration with standardized silver nitrate solution. A correction is made for the inorganic chlorine content of the sample, determined by the met
33、hod 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 better. 5.1 Glacial acetic acid. 5.2 2-Butoxyethanol (ethylene glycol monobutyl ether), stored in a brown bottle in the dark. WA
34、RNING 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 value is a volume fraction of 5 105. 5.3 2-Butanone (methyl ethyl ketone). 5.4 Methanol. WARNING Methanol is toxic. Avoid inhalatio
35、n 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 resins); in methanol (for glycidyl esters). Dissolve 120 g of sodium hydroxide in 75 ml of water plus sufficient 2-butoxyethanol
36、(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 Preparation 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
37、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 ml of glacial acetic acid (5.1). Then titrate potentiometrically with the silver nitrate solution prepared in 5.7.1. Conduct a b
38、lank test in the same way, leaving out the sodium chloride. EN ISO 21627-2:2009 (E) DIN EN ISO 21627-2:2010-01 65.7.3 Calculation of concentration Calculate the concentration using the following equation, rounding the result to three significant figures: ()200,00558,5mcVV=where c2is the concentratio
39、n 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 sodium chloride (g/mol); V is the volume of silver nitrate solution used in the titration, expressed in millilitres (ml); V0is t
40、he 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 in the dark. 6 Apparatus Usual laboratory apparatus, plus the following: 6.1 Potentiometric-titration apparatus, comprising a suitable potentiomete
41、r or autotitrator equipped with a glass-silver/silver chloride electrode system, titration stand and 10 ml microburette. 6.2 Analytical balance, accurate 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
42、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 stopper. 6.9 Reflux condenser. 6.10 Magnetic stirrer, with a PTFE (polytetrafluoroethylene) coated stirring bar. 7 Procedure 7.1 Epoxy resins 7.1.1 Weig
43、h, 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-butoxyethanol (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 r
44、oom temperature EN ISO 21627-2:2009 (E) DIN EN ISO 21627-2:2010-01 7and pipette 25 ml of sodium hydroxide solution in 2-butoxyethanol (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 short
45、er saponification time of 30 min is permissible if it can be shown to give similar results. This shall be recorded in the test report. 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
46、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 the 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, otherwis
47、e lower values might be obtained. 7.1.5 Carry out a blank test at the same time as the determination, following the same procedure and 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
48、 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 inor
49、ganic chlorine content of the sample in accordance with the method specified in ISO 21627-1. 7.2 Glycidyl esters 7.2.1 Glycidyl esters shall be pretreated by one of the following two methods: a) method A, using a beaker; b) method B, using a conical flask and reflux condenser. NOTE Method B is preferred for reasons of safety and hygiene. 7.2.2 Method A: 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 methanolic sodium hydroxide s
