BS EN ISO 21627-1-2009 Plastics - Epoxy resins - Determination of chlorine content - Inorganic chlorine《塑料 环氧树脂 氯含量的测定 无机氯》.pdf

1、BS EN ISO21627-1:2009ICS 83.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Epoxyresins Determination ofchlorine contentPart 1: Inorganic chlorine (ISO21627-1:2009)This British Standardwas published under theauthority of the StandardsPolicy and St

2、rategyCommittee on 31 October2009 BSI 2009ISBN 978 0 580 62856 6Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21627-1:2009National forewordThis British Standard is the UK implementation of EN ISO21627-1:2009. It supersedes BS EN ISO 21627-1:2003 which iswithdrawn.The UK partic

3、ipation 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 corr

4、ect application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN 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 - Pa

5、rt 1: Inorganic chlorine (ISO 21627-1:2009) Plastiques - Rsines poxydes - Dtermination de la teneur en 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 approve

6、d 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 alteration. Up-to-date lists and bibliographical references concerning such national st

7、andards 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 member into its own language and notifie

8、d 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, Italy, Latvia, Lithuania, Luxembourg, Malta

9、, 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-1000 Brussels 2009 CEN All rights of exploi

10、tation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21627-1:2009: EBS EN ISO 21627-1:2009EN ISO 21627-1:2009 (E) 3 Foreword This document (EN ISO 21627-1:2009) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical C

11、ommittee 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 national standards shall be withdrawn at the lat

12、est 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 EN ISO 21627-1:2003. According to the CEN/

13、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, Iceland, Ireland, Italy, Latvia, Lithuania, Lu

14、xembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21627-1:2009 has been approved by CEN as a EN ISO 21627-1:2009 without any modification. BS EN ISO 21627-1:2009ISO 21627-1:2009(E

15、) 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 results3 9 Precision 4 10 Test report4 Bibliography5 BS EN ISO 21627-1:2009ISO 21627-1:2009(E

16、) 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 technical committees. Each member body inte

17、rested 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 closely with the International Electrotechnica

18、l 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 International Standards adopted by the t

19、echnical 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 document may be the subject of patent rights. I

20、SO shall not be held responsible for identifying any or all such patent rights. ISO 21627-1 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 21627-1:2002), which has been technically

21、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 21627-1:2009ISO 21627-1:2009(E) ISO 2009 All rights reserved vIntroduc

22、tion 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 chemical activities differ significantly, so d

23、ifferent 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 called ionic chlorine). Part 2: Easily sap

24、onifiable 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 1-chloro-2-glycidylether (chloromethyl d

25、erivative) 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 impurities to be measured. For analytical met

26、hods 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 derivative) BS EN ISO 21627-1:2009BS EN ISO 21627-

27、1:2009INTERNATIONAL STANDARD ISO 21627-1:2009(E) ISO 2009 All rights reserved 1Plastics Epoxy resins Determination of chlorine content Part 1: Inorganic chlorine SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not pur

28、port 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 fo

29、r 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 dated

30、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 follo

31、wing 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. BS EN ISO 2162

32、7-1:2009ISO 21627-1:2009(E) 2 ISO 2009 All rights reserved5 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

33、(methyl ethyl ketone) 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

34、 (0,1 mol/l). Put 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

35、 1 l. Pipette 5 ml 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

36、 of concentration 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

37、 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 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 bo

38、ttle in the dark. BS EN ISO 21627-1:2009ISO 21627-1:2009(E) ISO 2009 All rights reserved 36 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 s

39、tand and 10 ml microburette. 6.2 Analytical 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

40、 Weigh, to the nearest 0,1 mg, 10 g of 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)

41、and adjust its position so that the electrodes (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.

42、 Adjust the speed of the stirrer to give 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 re

43、gions between points of inflection, where 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,

44、02 ml. 7.5 Continue the titration until 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,

45、keep the electrodes immersed in water. 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 solu

46、tion required to reach the end point. 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 inorgani

47、c chlorine content of the sample, expressed in milligrams per kilogram (mg/kg); BS EN ISO 21627-1:2009ISO 21627-1:2009(E) 4 ISO 2009 All rights reservedV1is 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

48、 nitrate solution used in the blank test, expressed in millilitres (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

49、 the first decimal place. 9 Precision The precision of this 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 repeatability standard deviation or the reproducibility standard deviation. Table 1 Precision of the method Inorganic chlorine content, w1(Cl) mg/kg Repeatability,