DIN EN ISO 21627-1-2010 Plastics - Epoxy resins - Determination of chlorine content - Part 1 Inorganic chlorine (ISO 21627-1 2009) German version EN ISO 21627-1 2009《塑料 环氧树脂 氯含量的测定.pdf

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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“1565188www

2、.din.deDDIN EN ISO 21627-1Plastics Epoxy resins - Determination of chlorine content Part 1: Inorganic chlorine (ISO 21627-1:2009)English version of DIN EN ISO 21627-1:2010-01Kunststoffe Epoxidharze - Bestimmung des Chlorgehaltes Teil 1: Anorganisches Chlor (ISO 21627-1:2009)Englische Fassung DIN EN

3、ISO 21627-1:2010-01SupersedesDIN EN ISO 21627-1:2004-05www.beuth.deDocument comprises pages11DIN EN ISO 21627-1:2010-01 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 “Plastic

4、s”, (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 a

5、s follows: ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN ISO 21627-1:2004-05 as follows: a) ISO 5725-2 has been transferred from “2 Normative references” to Bibliography. b) Under “Solution of silver nitrate in 2-propanol, 0,002 mol/l” (5.4), the equation in subclause 5.4.3 “Cal

6、culation 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 5.4.3 “Calculation of concentration” and 8 “Expression of results”, the gram equivalent of sodium chloride and of chlorine respectively is given. d) In cla

7、use 6 “Apparatus”, the specifications relating to the potentiometric-titration apparatus (6.1) have been rendered more precise. e) In clause 6 “Apparatus”, a new item 6.6 “Magnetic stirrer” has been added. f) In clause 9 “Precision”, the last sentence relating to the description of the materials use

8、d in the interlaboratory trial has been deleted. g) The standard has been editorially revised. Previous editions DIN EN ISO 11376: 2002-04 DIN EN ISO 21627-1: 2004-05 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods 2 EUROP

9、EAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21627-1 September 2009 ICS 83.080.10 Supersedes EN ISO 21627-1:2003English Version Plastics - Epoxy resins - Determination of chlorine content - Part 1: Inorganic chlorine (ISO 21627-1:2009) Plastiques - Rsines poxydes - Dtermination de la teneur e

10、n chlore - Partie 1: Chlore inorganique (ISO 21627-1:2009) Kunststoffe - Epoxidharze - Bestimmung des Chlorgehaltes -Teil 1: Anorganisches Chlor (ISO 21627-1:2009) This European Standard was approved by CEN on 19 August 2009. CEN members are bound to comply with the CEN/CENELEC Internal Regulations

11、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 be obtained on application to the CEN Management Centre or to any CEN member. This Europea

12、n 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 Management Centre has the same status as the official versions. CEN members are the natio

13、nal standards bodies of Austria, Belgium, Bulgaria, Cyprus, 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 U

14、nited 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 any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21627

15、-1:2009: EContents Page Foreword . .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 results7 9 Precision 8 10 Test report8 Bibliography9 .EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 2Foreword

16、This document (EN ISO 21627-1:2009) has been 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

17、 an identical text or by endorsement, at the 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

18、held responsible for identifying any or all such patent rights. This document supersedes EN ISO 21627-1:2003. 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,

19、Cyprus, 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 the United Kingdom. Endorsement notice The text of IS

20、O 21627-1:2009 has been approved by CEN as a EN ISO 21627-1:2009 without any modification. EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 3Introduction In producing epoxy resins based on epichlorohydrin, impurities containing chlorine may be formed. These are shown below. Since these impurities

21、could impair the final properties of the cured 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 chlori

22、des which occur as impurities in epoxy resins 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

23、 chlorine, consisting mainly of all saponifiable 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 th

24、e 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 impurities other than those shown below, see ISO 4615. Typical types of inorganic and organic chlorine impurity are shown below: Inorganic c

25、hlorine (or ionic chlorine) 1,2-Chlorohydrin 1,3-Chlorohydrin 1-Chloro-2-glycidylether (chloromethyl derivative) EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 4SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not

26、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 ISO 21627 specifies a direct potentiometric method

27、 for the determination of inorganic chlorine in epoxy resins, also called “ionic chlorine”. The inorganic chlorine content is expressed in milligrams per kilogram of epoxy resin. 2 Normative references The following referenced documents are indispensable for the application of this document. For dat

28、ed 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 3 Terms and definitions For the purposes of this document, the fo

29、llowing terms and definitions apply. 3.1 inorganic chlorine ionic chlorine amount of chlorine present in a resin as Cl4 Principle A test portion is dissolved in a suitable solvent and the inorganic chlorine determined by potentiometric titration with standardized silver nitrate solution. EN ISO 2162

30、7-1:2009 (E) DIN EN ISO 21627-1:2010-01 55 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 Acetone. In some cases, acetone may not dissolve the resin. In such cases, use butanone (methyl ethyl ket

31、one) or THF (tetrahydrofuran) or another suitable solvent and record the solvent used in the test report. 5.2 2-Propanol. 5.3 Glacial acetic acid. 5.4 Solution of silver nitrate in 2-propanol, 0,002 mol/l. 5.4.1 Preparation Dissolve 17 g of silver nitrate in water and make up to 1 l (0,1 mol/l). Put

32、 20 ml of this aqueous 0,1 mol/l silver nitrate solution in a 1 l graduated flask and dilute to 1 l with 2-propanol (5.2). 5.4.2 Standardization Weigh, to the nearest 0,1 mg, 115 mg to 120 mg of sodium chloride, previously dried at 500 C to 600 C, dissolve it in water and make up to 1 l. Pipette 5 m

33、l of this solution into a 200 ml beaker and add 100 ml of acetone (5.1) and 2 ml of glacial acetic acid (5.3). Then titrate potentiometrically with the silver nitrate solution prepared in 5.4.1. Conduct a blank test in the same way, leaving out the sodium chloride. 5.4.3 Calculation of concentration

34、 Calculate the concentration, to three significant figures, using the following equation: ()100,00558,5mcVV=where c1is 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 equival

35、ent 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). 5.4.4 Storage Store the silver nitrate solution in a brown bottle in the dark.

36、 EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 66 Apparatus Usual laboratory apparatus, plus the following: 6.1 Potentiometric-titration apparatus, comprising a suitable potentiometer equipped with a glass-silver/silver chloride electrode system, titration stand and 10 ml microburette. 6.2 Anal

37、ytical balance, accurate to 0,1 mg. 6.3 Beaker, of capacity 200 ml. 6.4 Graduated glass cylinder, of capacity 100 ml. 6.5 Pipettes, of capacities 1 ml, 2 ml and 5 ml. 6.6 Magnetic stirrer, with a PTFE (polytetrafluoroethylene) coated stirring bar. 7 Procedure 7.1 Weigh, to the nearest 0,1 mg, 10 g o

38、f sample into a 200 ml beaker (6.3). Add 100 ml of acetone (5.1) and dissolve the test portion at room temperature, using a magnetic stirrer (6.6). 7.2 Add 2 ml of water and 1 ml of glacial acetic acid (5.3). 7.3 Place the beaker on the titration stand (see 6.1) and adjust its position so that the e

39、lectrodes (see 6.1) are about half immersed. Fill the microburette with 0,002 mol/l silver nitrate solution (5.4), then place the burette in position on the titration stand so that the tip extends approximately 10 mm below the surface of the liquid in the beaker. Adjust the speed of the stirrer to g

40、ive vigorous stirring without splashing. Record the initial burette and meter (cell potential) readings. 7.4 Add small amounts of silver nitrate solution and, after waiting until the potential reaches a constant value, record the burette and meter readings. In regions between points of inflection, w

41、here the change in potential is small for each increment of silver nitrate solution, add volumes of up to 0,1 ml. Where the rate of change of the cell potential becomes higher than 5 mV per 0,02 ml, reduce the increments of silver nitrate solution to less than 0,02 ml. 7.5 Continue the titration unt

42、il the rate of change of cell potential again becomes lower than 2 mV per 0,02 ml of silver nitrate solution. Remove the titrated solution, rinse the electrodes well with water, wipe with a dry cloth and burnish lightly with fine emery cloth. Between titrations, keep the electrodes immersed in water

43、. 7.6 Plot the cumulative volumes of added silver nitrate solution against the cell potential. Take as the end point the middle of the steepest part of the curve (the inflection point). Read from the plot, to the nearest 0,01 ml, the volume of silver nitrate solution required to reach the end point.

44、 7.7 Conduct a blank test at the same time as the determination, following the same procedure. 8 Expression of results Calculate the inorganic chlorine content of the sample using the following equation: ()12 11035,5 1000(Cl )VV cwm = where w1(Cl) is the inorganic chlorine content of the sample, exp

45、ressed in milligrams per kilogram (mg/kg); EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 7V1is the volume of silver nitrate solution (5.4) 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 mi

46、llilitres (ml); c1is the concentration of the silver nitrate solution, calculated in accordance with 5.4.3 (mol/l); 35,5 is the gram equivalent of chlorine (g/mol); m0is the mass of the test portion, expressed in grams (g). Round the result to the first decimal place. 9 Precision The precision of th

47、is method was determined from an interlaboratory trial involving 10 laboratories and three levels. The trial was organized and the resulting data analysed in accordance with ISO 5725-2. Data from all 10 laboratories contained outliers. These outliers were not included in the calculation of the repea

48、tability standard deviation or the reproducibility standard deviation. Table 1 Precision of the method Inorganic chlorine content, w1(Cl) mg/kg Repeatability, srReproducibility, sRw1(Cl) 1 0,05 0,13 1 u w1(Cl) 3 0,14 0,27 3 u w1(Cl) u 5 0,25 0,55 sris the repeatability (within-laboratory) standard d

49、eviation; sRis the reproducibility (between-laboratory) standard deviation. 10 Test report The test report shall include the following information: a) a reference to this part of ISO 21627, i.e. ISO 21627-1; b) all details necessary for identification of the sample; c) the solvent used, if different from that indicated in 5.1 (acetone); d) the test results; e) the date of the test; f) any other relevant information. EN ISO 21627-1:2009 (E) DIN EN ISO 21627-1:2010-01 8Bibliography 1 ISO 4615, Plastics Unsaturated polyesters and epoxide r