BS-EN-ISO-6744-2-2004 BS-6782-16.2-2000.pdf

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1、BRITISH STANDARD BS EN ISO 6744-2:2004 BS 6782-16.2:2000 Incorporating Corrigendum No. 1 and Amendment No. 1 to BS 6782-16.2:2000 (Amendment No. 1 renumbers the BS as BS EN ISO 6744-2:2004) Binders for paints and varnishes Alkyd resins Part 2: Determination of phthalic anhydride content The European

2、 Standard EN ISO 6744-2:2004 has the status of a British Standard ICS 87.060.20 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 6744-2:2004 This British Standard, having been prepared under the direction of the Sector Committee f

3、or Materials and Chemicals, was published under the authority of the Standards Committee on 14 July 2004 BSI 14 July 2004 ISBN 0 580 34302 2 National foreword This British Standard is the official English language version of EN ISO 6744-2:2004. It is identical with ISO 6744-2:1999. The UK participat

4、ion in its preparation was entrusted to Technical Committee STI/3, Paint media and related products, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement internationa

5、l or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to

6、include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any e

7、nquiries 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. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO forewor

8、d page, the ISO title page, pages ii and iii, a blank page, pages 1 to 4, the Annex ZA page and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments 10884 Corrigendum No. 1 December 20

9、00Correction to identifier 1523914 July 2004Implementation of the European Standard Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 6744-2 May 2004 ICS 87.060.20 English version Binder

10、s for paints and varnishes - Alkyd resins - Part 2: Determination of phthalic anhydride content (ISO 6744-2:1999) Liants pour peintures et vernis - Rsines alkydes - Partie 2: Dtermination de la teneur en anhydride phtalique (ISO 6744-2:1999) Bindemittel fr Beschichtungsstoffe - Alkydharze - Teil 2:

11、Bestimmung des Gehaltes an Phthalsureanhydrid (ISO 6744-2:1999) This European Standard was approved by CEN on 8 April 2004. 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 wit

12、hout any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language ma

13、de by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany,

14、Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Ce

15、ntre: rue de Stassart, 36 B-1050 Brussels 2004 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 6744-2:2004 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI I NESO 76-44

16、:22( 400E) 2 Foreword The text of ISO 6744-2:1999 has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 6744-2:2004 by Technical Committee CEN/TC 139 “Paints and varnishes“, the secretar

17、iat of which is held by DIN. 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 November 2004, and conflicting national standards shall be withdrawn at the latest by November 2004. According to the C

18、EN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembour

19、g, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 6744-2:1999 has been approved by CEN as EN ISO 6744-2:2004 without any modifications. NOTE Normative references to International Standards are listed

20、 in Annex ZA (normative). EN ISO 67442:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 6744-2:1999(E) OSI 9991 INTERNATIONAL STANDARD ISO 6744-2 First edition 1999-12-01 Binders for paints and varnishes Alkyd resins

21、 Part 2: Determination of phthalic anhydride content Liants pour peintures et vernis Rsines alkydes Partie 2: Dtermination de la teneur en anhydride phtalique EN ISO 67442:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii EN ISO 67442:

22、2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO -44762:(9991)E ISO 9991 All irhgts seredevriii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodi

23、es). 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 right to be represented on that committee. International organizations, governmental and

24、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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, P

25、art 3. Draft International 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. Attention is drawn to the possibility that some of the elements of

26、 this part of ISO 6744 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 6744-2 was prepared by Technical Committee ISO/TC 35,Paints and varnishes, Subcommittee SC 10,Test methods for binders for paints an

27、d varnishes. Together with the other parts (see below), this part of ISO 6744 cancels and replaces ISO 6744:1984, which has been technically revised. ISO 6744 consists of the following parts, under the general titleBinders for paints and varnishes Alkyd resins: ?Part 1: General methods of test ?Part

28、 2: Determination of phthalic anhydride content ?Part 3: Determination of unsaponifiable matter content ?Part 4: Determination of fatty acid content EN ISO 67442:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI blank EN ISO 67442:2004 Li

29、censed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTENRATIONAL TSANDADRISO -44762:(9991)E ISO 9991 All irhgts seredevr1 Binders for paints and varnishes Alkyd resins Part 2: Determination of phthalic anhydride content 1Scope This part of ISO 67

30、44 specifies a method for determining the phthalic anhydride content of alkyd resins. It is only applicable to those alkyd resins which contain only orthophthalic acid as the polybasic acid. It is not applicable to modified alkyd resins (see 3.2 of ISO 6744-1:1999) or to resins containing benzoic ac

31、id. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 6744. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreement

32、s based on this part of ISO 6744 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of curre

33、ntly valid International Standards. ISO 3681:1996,Binders for paints and varnishes Determination of saponification value Titrimetric method. ISO 3696:1987,Water for analytical laboratory use Specification and methods of test. ISO 6744-1:1999,Binders for paints and varnishes Alkyd resins Part 1: Gene

34、ral methods of test. ISO 6744-3:1999,Binders for paints and varnishes Alkyd resins Part 3: Determination of unsaponifiable matter content. ISO 6744-4:1999,Binders for paints and varnishes Alkyd resins Part 4: Determination of fatty acid content. ISO 15528:1),Paints, varnishes and raw materials for p

35、aints and varnishes Sampling. 3Principle A test portion is saponified with potassium hydroxide solution. The potassium phthalate precipitate which forms is filtered, dried and weighed. The filtrate is reserved for the subsequent determinations of unsaponifiable matter and fatty acid contents. 1) To

36、be published. (Revision of ISO 842:1984 and ISO 1512:1991) EN ISO 67442:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO -44762:(9991)E 2 ISO 9991 All irhgts seredevr 4Reagents During the analysis, use only reagents of recognized ana

37、lytical grade and only water of at least grade 3 purity as defined in ISO 3696. 4.1Toluene. 4.2Solvent mixture, consisting of 1 part by volume of toluene and 1 part by volume of absolute ethanol. Alternatively, a mixture of 1 part by volume of diethyl ether and 1 part by volume of absolute ethanol m

38、ay be used. 4.3Potassium hydroxide, approximately 28 g/l solution in absolute ethanol, clear and free from sediment. 5Apparatus Ordinary laboratory apparatus and glassware, together with the following: 5.1Conical flask, of capacity about 250 ml, with ground-glass joint. 5.2Reflux condenser, with gro

39、und-glass joint, fitting on the conical flask (5.1) and the drying tube (5.3). 5.3Drying tube, filled with anhydrous calcium chloride, fitting on the reflux condenser (5.2). 5.4Hotplate, fitted with a magnetic stirrer. 5.5Sintered-glass filter crucible, diameter of the plate 30 mm, pore diameter 15

40、?m to 40 ?m. 5.6Desiccator, containing silica gel as the desiccant. 5.7Weighing bottle. 5.8Drying oven, capable of being maintained at approximately 140 C. 6Sampling Take a representative sample of the product to be tested, as described in ISO 15528. 7Procedure 7.1Number of determinations Carry out

41、the determination in duplicate. 7.2Test portion Weigh, to the nearest 1 mg, a mass (m0) of the resin or the resin solution containing not more than 2 g of fatty acid (see ISO 6744-4) into the conical flask (5.1). NOTEThe mass of resin to be taken will normally be 3 g to 5 g. 7.3Determination Dissolv

42、e the test portion (see 7.2) in 10 ml of toluene (4.1) in the conical flask. Add 100 ml of potassium hydroxide solution (4.3), fit the reflux condenser (5.2) on to the conical flask and fit the drying tube (5.3) on to the condenser. EN ISO 67442:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon N

43、ov 20 03:03:20 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO -44762:(9991)E ISO 9991 All irhgts seredevr3 Heat the contents of the flask to boiling and maintain at the boiling point under reflux for 2 h, while stirring (see note). Allow the flask to cool to ambient temperature, rinse the condenser

44、with some solvent and filter the solution through the weighed sintered-glass filter crucible (5.5). Reserve the filtrate for the determination of the unsaponifiable matter in accordance with ISO 6744-3. Wash the potassium phthalate precipitate as rapidly as possible several times with solvent mixtur

45、e (4.2). Make sure that the precipitate is continuously covered with the solvent mixture and only becomes exposed after the final washing. Afterwards, the precipitate may be placed in an oven maintained at 100 C for 1 min to 2 min to facilitate evaporation of the solvents. Dry the precipitate in the

46、 desiccator (5.6) under vacuum until the difference between the results of two consecutive weighings is not greater than 0,1 %, calculated on the basis of the lower value. Weigh the precipitate to the nearest 1 mg (m1). As the precipitate is hygroscopic, transfer the crucible and the precipitate imm

47、ediately after drying to the weighing bottle (5.7). Close the weighing bottle and weigh the precipitate to the nearest 1 mg. Dry the precipitate in the drying oven (5.8) at approximately 140 C until the difference between the results of two consecutive weighings is not greater than 0,1 %, calculated

48、 on the basis of the lower value. Weigh the residue to the nearest 1 mg (m2). NOTENormally, saponification is complete after 2 h. The completeness of saponification can be checked by determining the saponification value under more severe conditions which can be achieved by the use of a longer saponi

49、fication time, a more concentrated potassium hydroxide solution or a higher-boiling alcohol as solvent (see ISO 3681). 8Expression of results Calculate the phthalic anhydride content wp, expressed as a percentage by mass, by the equations w m m p ? ? 1 0 514 , (1) and w m m p ? ? 2 0 611 , (2) where m0is the mass, in grams, of the test portion (see note to 7.2); m1is the mass, in grams, of the precipitate after drying in

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