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 BS EN ISO 6744-2:2004 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee on 14 July 2004 BSI
3、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 participation in its preparation was entrusted to Technical Committee STI/3, Paint media and related products, which ha
4、s 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 international or European publications referred to in this document may be found in the BSI Catalogue under the section e
5、ntitled “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 include all the necessary provisions of a contract. Users are responsible for its correct application. Compli
6、ance 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 enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related
7、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 foreword page, the ISO title page, pages ii and iii, a blank page, pages 1 to 4, the Annex ZA page and a back cover.
8、 The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 10884 Corrigendum No. 1 December 2000 Correction to identifier 15239 14 July 2004 Implementation of the European StandardEUROPEANSTANDARD NORME
9、EUROPENNE EUROPISCHENORM ENISO67442 May2004 ICS87.060.20 Englishversion BindersforpaintsandvarnishesAlkydresinsPart2: Determinationofphthalicanhydridecontent(ISO67442:1999) LiantspourpeinturesetvernisRsinesalkydesPartie2: Dterminationdelateneurenanhydridephtalique(ISO 67442:1999) BindemittelfrBeschi
10、chtungsstoffeAlkydharzeTeil2: BestimmungdesGehaltesanPhthalsureanhydrid(ISO 67442:1999) ThisEuropeanStandardwasapprovedbyCENon8April2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalt
11、eration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberi
12、ntoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Po
13、land,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnational
14、Members. Ref.No.ENISO67442:2004EINESO7644:22(400E) 2 Foreword ThetextofISO67442:1999hasbeenpreparedbyTechnicalCommitteeISO/TC35“Paintsand varnishes”oftheInternationalOrganizationforStandardization(ISO)andhasbeentakenover asENISO67442:2004byTechnicalCommitteeCEN/TC139“Paintsandvarnishes“,the secretar
15、iatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyNovember2004,andconflictingnational standardsshallbewithdrawnatthelatestbyNovember2004. AccordingtotheCEN/CENELECInternalRegulations,thenationalstanda
16、rdsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary, Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland, Portugal,Slovakia,Slovenia,Spain,Sweden,Swit
17、zerlandandUnitedKingdom. Endorsementnotice ThetextofISO67442:1999hasbeenapprovedbyCENasENISO67442:2004withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinAnnexZA(normative). ENISO67442:2004Reference number ISO 6744-2:1999(E) OSI 9991 INTERNATIONAL STANDARD ISO 6744-2
18、First edition 1999-12-01 Binders for paints and varnishes Alkyd resins Part 2: Determination of phthalic anhydride content Liants pour peintures et vernis Rsines alkydes Partie 2: Dtermination de la teneur en anhydride phtalique ENISO67442:2004ii ENISO67442:2004ISO -44762:(9991)E ISO 9991 All irhgts
19、 seredevr iii Foreword 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 interested in a subject
20、 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 Electrotechnical Commission (IEC)
21、on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internatio
22、nal 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 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. Internat
23、ional Standard ISO 6744-2 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 10, Test methods for binders for paints and varnishes. Together with the other parts (see below), this part of ISO 6744 cancels and replaces ISO 6744:1984, which has been technically revise
24、d. ISO 6744 consists of the following parts, under the general title Binders for paints and varnishes Alkyd resins: Part 1: General methods of test Part 2: Determination of phthalic anhydride content Part 3: Determination of unsaponifiable matter content Part 4: Determination of fatty acid content E
25、NISO67442:2004blank ENISO67442:2004INTENRATIONAL TSANDADR ISO -44762:(9991)E ISO 9991 All irhgts seredevr 1 Binders for paints and varnishes Alkyd resins Part 2: Determination of phthalic anhydride content 1 Scope This part of ISO 6744 specifies a method for determining the phthalic anhydride conten
26、t 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 acid. 2 Normative references The following normative documents contai
27、n 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 agreements based on this part of ISO 6744 are encouraged to investigate the
28、 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 currently valid International Standards. ISO 3681:1996, Binders for pai
29、nts 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: General methods of test. ISO 6744-3:1999, Binders for paints and va
30、rnishes 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 paints and varnishes Sampling. 3P r i n c i p l e A test po
31、rtion 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 be published. (Revision of ISO 842:1984 and ISO 15
32、12:1991) ENISO67442:2004ISO -44762:(9991)E 2 ISO 9991 All irhgts seredevr 4 Reagents During the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity as defined in ISO 3696. 4.1 Toluene. 4.2 Solvent mixture, consisting of 1 part by volume of toluene and
33、 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 may be used. 4.3 Potassium hydroxide, approximately 28 g/l solution in absolute ethanol, clear and free from sediment. 5 Apparatus Ordinary laboratory apparat
34、us and glassware, together with the following: 5.1 Conical flask, of capacity about 250 ml, with ground-glass joint. 5.2 Reflux condenser, with ground-glass joint, fitting on the conical flask (5.1) and the drying tube (5.3). 5.3 Drying tube, filled with anhydrous calcium chloride, fitting on the re
35、flux condenser (5.2). 5.4 Hotplate, fitted with a magnetic stirrer. 5.5 Sintered-glass filter crucible, diameter of the plate 30 mm, pore diameter 15 mt o4 0 m. 5.6 Desiccator, containing silica gel as the desiccant. 5.7 Weighing bottle. 5.8 Drying oven, capable of being maintained at approximately
36、140 C. 6S a m p l i n g Take a representative sample of the product to be tested, as described in ISO 15528. 7 Procedure 7.1 Number of determinations Carry out the determination in duplicate. 7.2 Test portion Weigh, to the nearest 1 mg, a mass (m 0 ) of the resin or the resin solution containing not
37、 more than 2 g of fatty acid (see ISO 6744-4) into the conical flask (5.1). NOTE The mass of resin to be taken will normally be 3 g to 5 g. 7.3 Determination Dissolve 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
38、reflux condenser (5.2) on to the conical flask and fit the drying tube (5.3) on to the condenser. ENISO67442:2004ISO -44762:(9991)E ISO 9991 All irhgts seredevr 3 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 fl
39、ask to cool to ambient temperature, rinse the condenser 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
40、as rapidly as possible several times with solvent mixture (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
41、 evaporation of the solvents. Dry the precipitate in the 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 (m 1 ). As the precipitate is
42、hygroscopic, transfer the crucible and the precipitate immediately 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 c
43、onsecutive weighings is not greater than 0,1 %, calculated on the basis of the lower value. Weigh the residue to the nearest 1 mg (m 2 ). NOTE Normally, saponification is complete after 2 h. The completeness of saponification can be checked by determining the saponification value under more severe c
44、onditions which can be achieved by the use of a longer saponification time, a more concentrated potassium hydroxide solution or a higher-boiling alcohol as solvent (see ISO 3681). 8 Expression of results Calculate the phthalic anhydride content w p , expressed as a percentage by mass, by the equatio
45、ns w m m p 1 0 514 , (1) and w m m p 2 0 611 , (2) where m 0 is the mass, in grams, of the test portion (see note to 7.2); m 1 is the mass, in grams, of the precipitate after drying in vacuum at ambient temperature (potassium phthalate monoethanolate); m 2 is the mass, in grams, of the residue after
46、 drying at 140 C (ethanol-free potassium phthalate); 51 ,4 is a factor to convert the mass of potassium phthalate monoethanolate to that of phthalic anhydride; 61 ,1 is a factor to convert the mass of anhydrous potassium phthalate to that of phthalic anhydride. Calculate the average of the two value
47、s and report this average value. NOTE If the difference between the results calculated by the two equations is greater than 2 % absolute, the method specified in this part of ISO 6744 is not suitable for the alkyd resin under test (see footnote c to Table 1 of ISO 6744-1:1999). The phthalic anhydride content shall be calculated on the basis of the resin or, for resin solutions, on the basis of the non-volatile matter content of the solution. ENISO67442:2004ISO -44762:(9991)E 4 ISO 9991 All irhgts seredevr 9 Test report The test report shall contain at least the following infor
