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1、BRITISH STANDARD BS EN ISO 9702:1999 Incorporating Amendment No. 1 to BS ISO 9702:1996 (renumbers the BS as BS EN ISO 9702:1999) Plastics Amine epoxide hardeners Determination of primary, secondary and tertiary amine group nitrogen content The European Standard EN ISO 9702:1998 has the status of a B
2、ritish Standard ICS 83.040.30 BS EN ISO 9702:1999 This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 April 1997 BSI 05-1999 ISBN 0 580 27213 3 National f
3、oreword This British Standard is the English language version of EN ISO 9702:1998. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: aid enquirers to understand the text; present
4、 to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be o
5、btained on request. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the
6、 BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summ
7、ary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, page 2, the ISO title page, page ii, pages 1 to 6 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated i
8、n the amendment table on the inside front cover. Amendments issued since publication Amd. No.DateComments 10346April 1999Implementation of the European Standard BS EN ISO 9702:1999 BSI 05-1999i Contents Page National foreword Inside front cover Foreword 2 Text of ISO 97021 ii blank EUROPEAN STANDARD
9、 NORME EUROPENNE EUROPISCHE NORM EN ISO 9702 August 1998 ICS 83.080.10 Descriptors: See ISO document English version Plastics Amine epoxide hardeners Determination of primary, secondary and tertiary amine group nitrogen content (ISO 9702:1996) Plastiques Durcisseurs pour rsines poxy Dtermination de
10、la teneur en azote des groupes amine primaire, secondaire, tertiaire (ISO 9702:1996) Kunstoffe Aminische Epoxidhrter Bestimmung von primren, sekundren und tertiren Amingruppen als Stickstoffgehalt (ISO 9702:1996) This European Standard was approved by CEN on 12 June 1998. CEN members are bound to co
11、mply 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 be obtained on application to the Central S
12、ecretariat 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 Central Secretariat has the same status as the o
13、fficial versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardizatio
14、n Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 9702:1998 E EN ISO 9702:1998 BSI 05-1999 2 Foreword T
15、he text of the International Standard from Technical Committee ISO/TC 61, Plastics, of the International Organization for Standardization (ISO) has been taken over as a European Standard by Technical Committee CEN/TC 249, Plastics, the Secretariat of which is held by IBN. This European Standard shal
16、l be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 1999, and conflicting national standards shall be withdrawn at the latest by February 1999. According to CEN/CENELEC Internal Regulations, the following countries are
17、 bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS
18、O 9702:1996 has been appoved by CEN as a European Standard without any modification. Contents Page Foreword 2 1Scope1 2Principle1 3Reagents2 4Apparatus3 5Procedure3 6Expression of results4 7Precision6 8Test report6 BS EN ISO 9702:1999 ii BSI 05-1999 Foreword ISO (the International Organization for S
19、tandardization) 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 subject for which a technical committee has been established has the ri
20、ght 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 (IEC) on all matters of electrotechnical standardization. Draft Intern
21、ational Standards adopted by the technical 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. International Standard ISO 9702 was prepared by Technical Committee ISO/TC 61, Plasti
22、cs, Subcommittee SC 12, Thermosetting materials. Descriptors: Plastics, epoxy resins, resin hardeners, amines, chemical analysis, determination of content, nitrogen, potentiometric methods. BS EN ISO 9702:1999 BSI 05-19991 1 Scope This International Standard specifies a method for the determination
23、of the primary, secondary and tertiary amine group nitrogen content of aliphatic or aromatic amine hardeners for epoxy resins. 2 Principle 2.1 Aliphatic amines 2.1.1 Determination of total amine group nitrogen content (XT) The total alkalinity is determined by potentiometric titration against hydrob
24、romic or perchloric acid in glacial acetic acid, as described by the following reactions: RNH2 + H+ F RNH3+ (RR9NH + H+ F (RR9) NH2+ (RRR)N + H+F (RRR)NH+ The results are expressed as percentage nitrogen. NOTE 1Perchloric acid is not suitable for use with amine hardeners such as N-aminoethylpiperazi
25、ne. 2.1.2 Determination of tertiary amine group nitrogen content (X3) The primary and secondary amine groups are converted into amide groups with acetic anhydride, as described by the following reactions: The tertiary amine group alkalinity is determined by potentiometric titration against hydrobrom
26、ic or perchloric acid in glacial acetic acid/acetic anhydride, as described by the following reaction: (RR9R0)NH + H+F (RR9R0)NH+ The results are expressed as percentage nitrogen. 2.1.3 Determination of primary amine group nitrogen content (XL1) The primary amine groups are reacted with a measured e
27、xcess of 2,4-pentanedione (acetylacetone) in N,N-di-methylformamide to form imines, as described by the following reaction: The excess acetylacetone is determined by potentiometric titration against potassium hydroxide (the reaction products of acetylacetone and primary amine groups are neutral unde
28、r these conditions). The results are expressed as percentage nitrogen. 2.1.4 Determination of secondary amine group nitrogen content (XL2) The secondary amine group nitrogen content is determined by calculating the difference between the total amine group nitrogen content and the sum of the primary
29、and tertiary amine group nitrogen contents. 2.2 Aromatic amines 2.2.1 Determination of total amine group nitrogen content (XT) The total alkalinity is determined by potentiometric titration against hydrobromic or perchloric acid in glacial acetic acid, as described by the following reactions: ArNH2+
30、 H+F ArNH3+ (ArAr9)NH + H+F (ArAr9)NH2+ (ArAr9Ar0)N + H+F (ArAr9Ar0)NH+ The results are expressed as percentage nitrogen. 2.2.2 Determination of tertiary amine group nitrogen content (X3) The primary and secondary amine groups are converted into amide groups with acetic anhydride as described by the
31、 following reactions: The tertiary amine group alkalinity is determined by potentiometric titration against hydrobromic or perchloric acid in glacial acetic acid/acetic anhydride, as described by the following reaction. (ArAr9Ar0)N + H+F (ArAr9Ar0)NH+ The results are expressed as percentage nitrogen
32、. 2.2.3 Determination of the sum of the secondary and tertiary amine group nitrogen contents (XR2 + 3) The primary amine groups are converted into Schiff bases by salicylaldehyde in glacial acetic acid, as described by the following reaction: RNH2+ (CH3CO)2O F RNHCOCH3+ CH3COOH (RR)NH + (CH3CO)2O F
33、(RR9)NCOCH3+ CH3COOH RNH2+ CH3COCH2COCH3F CH3CNRCH2COCH3+ H2O ArNH2+ (CH3CO)2O F ArNHCOCH3+ CH3COOH (ArAr9)NH + (CH3CO)2O F (ArAr9)NCOCH3+ CH3COOH ArNH2+ C6H4(OH)CHO F ArN = CHC6H4(OH) + H2O BS EN ISO 9702:1999 2 BSI 05-1999 With strongly basic amines, the secondary and tertiary amine group alkalini
34、ty is determined by potentiometric titration against hydrochloric acid in glacial acetic acid, as described by the following reactions: (ArAr)NH + H+F (ArAr)NH2+ (ArArAr)N + H+F (ArArAr)NH+ The results are expressed as percentage nitrogen. NOTE 2Weakly basic amines, such as 4,4-diamino-diphenylsulfo
35、ne, are titrated with hydrobromic or perchloric acid in glacial acetic acid. 2.2.4 Determination of primary amine group nitrogen content (XR1) The primary amine group nitrogen content is determined by calculating the difference between the total amine group nitrogen content and the sum of the second
36、ary and tertiary amine group nitrogen contents. 2.2.5 Determination of secondary amine group nitrogen content (XR2) The secondary amine group nitrogen content is determined by calculating the difference between the sum of the secondary and tertiary amine group nitrogen contents and the tertiary amin
37、e group nitrogen content. 3 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 3.1 Acetic acid, glacial. 3.2 Acetic anhydride. 3.3 2,4-Pentanedione (acetylacetone). 3.4 N,N-diamethylformamide. 3.5 Acetylacetone, 1,5
38、mol/l solution in N,N-dimethylformamide. Dissolve 15 ml of acetylacetone (3.3) in 90 ml of N,N-dimethylformamide (3.4). 3.6 Salicylaldehyde. 3.7 Ethan-1,2-diol (ethylene glycol). 3.8 Propan-2-ol. 3.9 Ethylene glycol/propan-2-ol mixed solvent Mix 500 ml of ethylene glycol (3.7) and 500 ml of propan-2
39、-ol (3.8). 3.10 Potassium hydrogen phthalate. 3.11 Hydrobromic acid, 250 g/l solution in acetic acid. 3.12 Perchloric acid, 70 % or 60 % solution in water. 3.13 Potassium hydroxide. 3.14 Hydrochloric acid, concentrated. 3.15 Sodium carbonate. 3.16 Hydrobromic acid, 0,1 mol/l standard volumetric solu
40、tion in glacial acetic acid. 3.16.1 Preparation Add 25 ml of hydrobromic acid (3.11) slowly to 100 ml of glacial acetic acid (3.1) in a 1 000 ml brown-glass volumetric flask (4.9) and stir carefully. Dilute to the mark with glacial acetic acid. 3.16.2 Standardization Weigh out, to the nearest 0,1 mg
41、, 0,1 g to 0,2 g of potassium hydrogen phthalate (3.10) and dissolve in 50 ml of glacial acetic acid (3.1). Titrate this solution potentiometrically against the solution of hydrobromic acid prepared in 3.16.1 (V1). Perform a blank test by titrating 50 ml of glacial acetic acid against the solution o
42、f hydrobromic acid prepared in 3.16.1 (V2). Calculate the concentration c1 of the hydrobromic acid solution, expressed in moles of HBr per litre to the nearest 0,001 mol HBr/l, using the equation where 3.17 Perchloric acid, 0,1 mol/l standard volumetric solution in glacial acetic acid. 3.17.1 Prepar
43、ation Mix 8,5 ml of 70 % perchloric acid (or 9,9 ml of 60 % perchloric acid) (3.12) with 500 ml of glacial acetic acid (3.1) in a 1 000 ml brown-glass volumetric flask (4.9). Add 30 ml (or 35 ml if 60 % perchloric acid was used) of acetic anhydride (3.2) and mix well. Dilute to the mark with glacial
44、 acetic acid. 3.17.2 Standardization Use the same procedure as that in 3.16.2, calculating the concentration using the same equation. In this case, c1 is the concentration of the perchloric acid solution prepared in 3.17.1. m0is the mass, in grams, of potassium hydrogen phthalate used; V1is the volu
45、me, in millilitres, of the solution of hydrobromic acid prepared in 3.16.1 required to reach the end point in the titration; V2is the volume, in millilitres of the above solution (3.16.1) required in the blank test. c1 1 000 m0 204,23 V1V2() -= BS EN ISO 9702:1999 BSI 05-19993 3.18 Potassium hydroxi
46、de, 0,5 mol/l standard volumetric solution in propan-2-ol. 3.18.1 Preparation Take 1 000 ml of propan-2-ol (3.8) in a round-bottomed flask and add 30 g of potassium hydroxide (3.13). Reflux for several hours to dissolve completely. Leave the solution in a carbon-dioxide-free atmosphere for a few day
47、s, then transfer the clear upper solution to a polyethylene bottle and keep it in the bottle equipped with a guard tube filled with soda lime. Take care that the solution does not touch a cork or rubber stopper or stopper grease, which may be saponified. 3.18.2 Standardization Weigh, to the nearest
48、0,1 mg, 0,5 g to 1,0 g of potassium hydrogen phthalate (3.10) and dissolve in 100 ml of water. Titrate this solution potentiometrically against the potassium hydroxide solution prepared in 3.18.1 (V3). Perform a blank test separately (V4). Calculate the concentration c2 of the potassium hydroxide so
49、lution, expressed in moles of KOH per litre to the nearest 0,001 mol KOH/l, using the equation where 3.19 Hydrochloric acid, 0,1 mol/l standard volumetric solution in mixed solvent. 3.19.1 Preparation Add 1 000 ml of the ethylene glycol/propan-2-ol mixed solvent (3.9) to 9 ml of concentrated hydrochloric acid (3.14). 3.19.2 Standardization Weigh out, to the nearest 0,1 mg, 0,13 g to 0,16 g of sodium carbonate (3.15) and dissolve in 100 ml of water. Titrate this solution potentiometrica