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!$Tn“1564975ww
2、w.din.deDDIN EN ISO 21627-3Plastics Epoxy resins - Determination of chlorine content Part 3: Total chlorine (ISO 21627-3:2009)English version of DIN EN ISO 21627-3:2010-01Kunststoffe Epoxidharze - Bestimmung des Chlorgehaltes Teil 3: Gesamtgehalt an Chlor (ISO 21627-3:2009)Englische Fassung DIN EN I
3、SO 21627-3:2010-01SupersedesDIN EN ISO 21627-3:2004-04www.beuth.deDocument comprises pages12DIN EN ISO 21627-3:2010-01 National foreword This standard has been prepared by Technical Committee ISO/TC 61 “Plastics” (Secretariat: ANSI, USA) in collaboration with Technical Committee CEN/TC 249 “Plastics
4、”, (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 Standard corresponding to the International Standard referred to in this document is as
5、 follows: ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN ISO 21627-3:2004-04 as follows: a) ISO 5725-2 has been transferred from “2 Normative references” to Bibliography. b) Under “Silver nitrate, 0,1 mol/l aqueous standard solution” (5.5), the equation in subclause 5.5.3 “Calcul
6、ation of concentration” has been modified in that the gram equivalent of sodium chloride (g/mol) is 58,5 (instead of 58,45) and the volume of silver nitrate solution used in the titration is V (instead of V1). c) In subclauses 5.5.3 “Calculation of concentration” and 8 “Expression of results”, the g
7、ram equivalent of sodium chloride and of chlorine respectively is given. d) Under “Silver nitrate, 0,01 mol/l aqueous standard solution” (5.6), subclauses 5.6.3 “Calculation of concentration” and 5.6.4 “Storage” have been added. e) In clause 6 “Apparatus”, a new item 6.11 “Magnetic stirrer” has been
8、 added. f) In clause 7 “Procedure”, the use of a magnetic stirrer has been included (7.2). g) In clause 8 “Expression of results”, the equation for the calculation of the total chlorine content has been modified in that the gram equivalent of chlorine (g/mol) is 35,5 (instead of 35,45), the volume o
9、f silver nitrate solution used in the blank is V2 (instead of V0) and the mass of the test portion is m0 (instead of m). h) In clause 9 “Precision”, the last sentence relating to the description of the materials used in the interlaboratory trial has been deleted. i) The standard has been editorially
10、 revised. Previous editions DIN EN ISO 21627-3: 2004-04 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21627-3 September 2009 ICS 83.080.10 Supersedes EN ISO 2162
11、7-3:2003English Version Plastics - Epoxy resins - Determination of chlorine content - Part 3: 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 - Tei
12、l 3: Gesamtgehalt an Chlor (ISO 21627-3:2009) This European Standard was approved by CEN on 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 alterat
13、ion. 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, French, German). A version in any other language made by transl
14、ation 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, Czech Republic, Denmark, Estonia, Finland, France, Germany
15、, 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Ma
16、nagement 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 21627-3:2009: EContents Page 1 Scope5 2 Normative references5 3 Terms and definitions .5 4 Principle .5 EN ISO 21627-3:2009
17、 (E) DIN EN ISO 21627-3:2010-01 2Foreword . .3 Introduction.4 1 Scope5 2 Normative references5 3 Terms and definitions .5 4 Principle .5 5 Reagents 6 6 Apparatus.7 7 Procedure.7 8 Expression of results8 9 Precision 8 10 Test report9 Bibliography10 .Foreword This document (EN ISO 21627-3:2009) has be
18、en prepared by Technical 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 t
19、he latest by March 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 al
20、l such patent rights. This document supersedes EN ISO 21627-3:2003. 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,
21、Finland, France, Germany, 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 21627-3:2009 has been approved by CEN as
22、 a EN ISO 21627-3:2009 without any modification. EN ISO 21627-3:2009 (E) DIN EN ISO 21627-3:2010-01 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 c
23、ured resins, it is 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 res
24、ins derived from epichlorohydrin: 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 saponi
25、fiable organic chlorine, 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 di
26、ffer, one of these 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-Chlorohydr
27、in 1,3-Chlorohydrin 1-Chloro-2-glycidylether (chloromethyl derivative) EN ISO 21627-3:2009 (E) DIN EN ISO 21627-3:2010-01 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 conce
28、rns, 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 amount of chlorine in epoxy
29、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, only the edition cited a
30、pplies. 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 and definitions apply. 3.
31、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 chlorine present in the test p
32、ortion 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 of the solution with si
33、lver nitrate solution. EN ISO 21627-3:2009 (E) DIN EN ISO 21627-3:2010-01 55 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 Diethylene glycol monobutyl ether. 5.2 Potassi
34、um 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 Preparation Dissolve 17 g of silver nitrate in
35、 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 beaker and add 100 ml of acetone (5.4) and 2
36、 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 Calculate the concentration, to three significant
37、 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 sodium chloride (g/mol); V is the volume of
38、 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 Silver nitrate, 0,01 mol/l aqueous standard s
39、olution. 5.6.1 Preparation Dissolve 1,7 g of silver nitrate in water and make up to 1 l. EN ISO 21627-3:2009 (E) DIN EN ISO 21627-3:2010-01 65.6.2 Standardization Weigh, to the nearest 0,1 mg, 584 mg of sodium chloride previously dried at 500 C to 600 C, dissolve it in water and make up to 1 l to gi
40、ve 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 5.6.1. Carry out a blank test in the same manner, omitting the
41、 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. 6 Apparatus Usual laboratory apparatus, plus the following: 6.
42、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 Volumetric flask, of capacity 1 l. 6.4 Hotplate or oil bath, capable of
43、 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, of capacity 200 ml. 6.11 Magnetic stirrer, with a PTFE (polytet
44、rafluoroethylene) 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 is less than 1 % or a test portion of a size such that it conta
45、ins 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 potassium hydroxide solution in 1,2-propanediol (5.2). Reflux the solut
46、ion on a hotplate or in an oil bath (6.4) for 10 min while stirring. EN ISO 21627-3:2009 (E) DIN EN ISO 21627-3:2010-01 77.4 Leave to cool, then pour 5 ml of acetone (5.4) down the reflux condenser. 7.5 Transfer the solution from the flask to a 200 ml beaker (6.10). Wash the inside of the flask thre
47、e 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 vigorous stirring without splashing. 7.7 Carry out the potentiometric titration with 0,
48、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 a blank test in the same way. 8 Expression of results Calculate the total chlorine
49、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 silver nitrate solution, calculated in accordance with 5.5.3 (mol/l); 35,5 is the gram equivalent of chlorine (g/mol); m
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