1、BRITISH STANDARD BS EN ISO 6744-3:2004 BS 6782-16.3:2000 Incorporating Corrigendum No. 1 and Amendment No. 1 to BS 6782-16.3:2000 (renumbers the BS as BS EN ISO 6744-3:2004) Binders for paints and varnishes Alkyd resins Part 3: Determination of unsaponifiable matter content The European Standard EN
2、ISO 6744-3:2004 has the status of a British Standard ICS 87.060.20 BS EN ISO 6744-3:2004 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 and comes into effect on 15 March
3、 2000 BSI 9 July 2004 ISBN 0 580 34303 0 National foreword This British Standard is the official English language version of EN ISO 6744-3:2004. It is identical with ISO 6744-3:1999. The UK participation in its preparation was entrusted to Technical Committee STI/3, Paint media and related products,
4、 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 international or European publications referred to in this document may be found in the BSI Catalogue under the
5、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 include all the necessary provisions of a contract. Users are responsible for its correct applicatio
6、n. 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 enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor
7、 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 foreword, the ISO title page, pages ii and iii, a blank page, pages 1 to 3, the Annex ZA page, an inside ba
8、ck cover 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. Date Comments 10885 Corrigendum No. 1 December 2000 Correction to identifier 15240 9 July 2004 Implementation of the European Stand
9、ardEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO67443 May2004 ICS87.060.20 Englishversion BindersforpaintsandvarnishesAlkydresinsPart3: Determinationofunsaponifiablemattercontent(ISO6744 3:1999) LiantspourpeinturesetvernisRsinesalkydesPartie3: Dterminationdelateneurenmatireinsaponifiable(ISO
10、67443:1999) BindemittelfrBeschichtungsstoffeAlkydharzeTeil3: BestimmungdesGehaltesanunverseifbarenBestandteilen (ISO67443:1999) ThisEuropeanStandardwasapprovedbyCENon8April2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardt
11、hestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nsla
12、tion undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuani
13、a,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandby
14、anymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO67443:2004EINESO7644:32(400E) 2 Foreword ThetextofISO67443:1999hasbeenpreparedbyTechnicalCommitteeISO/TC35“Paintsand varnishes”oftheInternationalOrganizationforStandardization(ISO)andhasbeentakenover asENISO67443:2004byTechnicalCommitteeCE
15、N/TC139“Paintsandvarnishes“,the secretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyNovember2004,andconflictingnational standardsshallbewithdrawnatthelatestbyNovember2004. AccordingtotheCEN/CENE
16、LECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, Cyprus,CzechRepublic,Denmark,Estonia,Finland,France,Germany,Greece,Hungary, Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland, Port
17、ugal,Slovakia,Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. Endorsementnotice ThetextofISO67443:1999hasbeenapprovedbyCENasENISO67443:2004withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinAnnexZA(normative). ENISO67443:2004Reference number ISO 6744-3:1999(E) OSI
18、 9991 INTERNATIONAL STANDARD ISO 6744-3 First edition 1999-12-01 Binders for paints and varnishes Alkyd resins Part 3: Determination of unsaponifiable matter content Liants pour peintures et vernis Rsines alkydes Partie 3: Dtermination de la teneur en matire insaponifiable ENISO67443:2004 iiENISO674
19、43:2004ISO -44763:(9991)E ISO 9991 All irhgts 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 committ
20、ees. 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 non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Int
21、ernational Electrotechnical Commission (IEC) 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 bo
22、dies 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 part of ISO 6744 may be the subject of patent rights. ISO shall not be held responsible for identi
23、fying any or all such patent rights. International Standard ISO 6744-3 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
24、 6744:1984, which has been technically revised. 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
25、Part 4: Determination of fatty acid content ENISO67443:20044002:34476OSINEINTENRATIONAL TSANDADR ISO -44763:(9991)E ISO 9991 All irhgts seredevr 1 Binders for paints and varnishes Alkyd resins Part 3: Determination of unsaponifiable matter content 1 Scope This part of ISO 6744 specifies a method for
26、 determining the unsaponifiable matter content of alkyd resins. It is always used in conjunction with ISO 6744-2, which describes the first step of the analysis. It is not applicable to modified alkyd resins (see 3.2 of ISO 6744-1:1999). 2 Normative references The following normative documents conta
27、in 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 th
28、e 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 3696:1987, Water for anal
29、ytical 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 6744-2:1999, Binders for paints and varnishes Alkyd resins Part 2: Determination of phthalic anhydride content. ISO 6744-4:1999, Binders for pa
30、ints 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 The unsaponifiable matter content of a saponified alkyd resin sample is determined by drying the filtrate obtained in
31、 ISO 6744-2 and extraction with diethyl ether or light petroleum ether to remove the fatty acids. The residue is weighed and the percentage is calculated based on the initial sample mass obtained from ISO 6744-2. 4 Reagents During the analysis, use only reagents of recognized analytical grade and on
32、ly water of at least grade 3 purity as defined in ISO 3696. 1) To be published. (Revision of ISO 842:1984 and ISO 1512:1991) ENISO67443:2004ISO -44763:(9991)E 2 ISO 9991 All irhgts seredevr 4.1 Diethyl ether, free from peroxides, to which a crystal of hydroquinone has been added (for the diethyl eth
33、er method specified in 7.2). 4.2 Light petroleum, boiling range 30 C to 50 C (for the light petroleum method specified in 7.3). NOTE In some countries, this solvent is known as “petroleum ether 30/50“. 4.3 Potassium hydroxide, 56 g/l aqueous solution. 4.4 Acetone. 4.5 Ethanol, 95 % (by volume). 5 Ap
34、paratus Ordinary laboratory apparatus and glassware, together with the following: 5.1 Separating funnels, of capacity 250 ml. 5.2 Distillation apparatus, with a rotary evaporator or water bath. 5.3 Drying oven, capable of being maintained at approximately 105 C. 6 Sampling Take a representative samp
35、le of the product to be tested, as described in ISO 15528. 7 Procedure 7.1 Number of determinations Carry out the determination in duplicate. NOTE When using the diethyl ether method (7.2), emulsions may be formed which are difficult to separate. In such cases, ethanol, saturated sodium chloride sol
36、ution or a few drops of dilute mineral acid may be added to break the emulsion. In certain cases, it may also be helpful to use the light petroleum method (7.3) instead of the diethyl ether method. 7.2 Diethyl ether method Vacuum-distill or evaporate the solvent from the filtrate obtained as describ
37、ed in ISO 6744-2:1999, subclause 7.3. Dissolve the residue in 25 ml of ethanol (4.5) and 50 ml of water and transfer to a separating funnel (5.1). Rinse the container with 50 ml of diethyl ether (4.1) and collect all the washings in the separating funnel. Stopper the separating funnel, shake and all
38、ow the layers to separate. Drain off the lower (aqueous) layer into a second separating funnel (5.1) and retain the other layer in the first separating funnel. Continue the extraction of the aqueous layer with two further 50 ml portions of diethyl ether. Combine all the ether extracts in the first s
39、eparating funnel and reserve the aqueous layer for the determination of the fatty acid content in accordance with ISO 6744-4. Wash the combined ether extracts with 25 ml portions of water until the pH of the washings is neutral. Add the washings to the aqueous layer obtained by the procedure describ
40、ed above. Evaporate the ether using a suitable apparatus (5.2), either under inert gas using a distillation apparatus with a rotary evaporator or, while observing all required safety precautions, over a water bath. If necessary, remove any water present by addition of acetone (4.4) and evaporating a
41、s above. ENISO67443:2004ISO 6744-3:1999(E) ISO 9991 All irhgts seredevr 3 Dry the residue in the drying oven (5.3) at approximately 105 C 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 residue to
42、the nearest 1 mg (m 3 ). 7.3 Light petroleum method Vacuum distill or evaporate the solvent from the filtrate obtained as described in ISO 6744-2:1999, subclause 7.3. Transfer the residue with about 100 ml of water to a separating funnel (5.1) and add 50 ml of light petroleum (4.2). Rinse the contai
43、ner with 50 ml of light petroleum and collect all the washings in the separating funnel. Stopper the separating funnel, shake and allow the layers to separate. Drain off the lower (aqueous) layer into a second separating funnel (5.1) and retain the other layer in the first separating funnel. Continu
44、e the extraction of the aqueous layer with two further 50 ml portions of light petroleum. Combine all the light petroleum extracts in the first separating funnel and reserve the aqueous layer for the determination of the fatty acid content in accordance with ISO 6744-4. Shake the combined light petr
45、oleum extracts with a mixture consisting of 15 ml of ethanol (4.5), 15 ml of water and 0,5 ml of potassium hydroxide solution (4.3), allow the layers to separate and drain off the lower (aqueous) layer. Wash the light petroleum extracts with 25 ml portions of water until the pH of the washings is ne
46、utral. Add all the aqueous washings to the aqueous layer obtained by the procedure described above. Evaporate the light petroleum using any suitable apparatus (5.2), and remove the water from the residue by addition of acetone (4.4) and evaporate as described above. Dry the residue in the drying ove
47、n (5.3) at approximately 105 C 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 residue to the nearest 1 mg (m 3 ). 8 Expression of results Calculate the unsaponifiable matter content w U , expresse
48、d as a percentage by mass, by the equation w m m U 3 0 100 where m 0 is the mass, in grams, of the test portion (see ISO 6744-2:1999, subclause 7.2); m 3 is the mass, in grams, of the residue. The unsaponifiable matter content shall be calculated on the basis of the resin or, for resin solutions, on the b
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