1、 DEUTSCHE NORMJune 2006DIN EN ISO 15023-2 ICS 83.080.20 Plastics Poly(vinyl alcohol) (PVAL) materials Part 2: Determination of properties (ISO 15023-2:2003) English version of DIN EN ISO 15023-2:2006-06 Kunststoffe Polyvinylalkohol (PVAL)-Formmassen Teil 2: Bestimmung von Eigenschaften (ISO 15023-2:
2、2003) Englische Fassung DIN EN ISO 15023-2:2006-06 Document comprises 21 pages No part of this standard may be reproduced without prior permission of DIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, has the exclusive right of sale for German Standards (DIN-N
3、ormen). English price group 11 www.din.de www.beuth.de !,o4q“11.06 9761778DIN EN ISO 15023-2:2006-06 2 National foreword This standard has been published in accordance with a decision taken by CEN/TC 249 to adopt, without alteration, International Standard ISO 15023-2 as a European Standard. The res
4、ponsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Technical Committee NA 054-02-08 AA Sonstige Thermoplast-Formmassen. The DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as follows: I
5、SO 976 DIN ISO 976 ISO 6587 DIN 53114 ISO 8130-1 DIN ISO 8130-1 ISO 12058-1 DIN EN ISO 12058-1 ISO 15023-1 DIN EN ISO 15023-1 National Annex NA (informative) Bibliography DIN 53114, Determining the conductivity of aqueous extracts of paper, board and pulp DIN EN ISO 12058-1, Plastics Determination o
6、f viscosity using a falling-ball viscometer Part 1: Inclined-tube method DIN EN ISO 15023-1, Plastics Poly(vinyl alcohol) (PVAL) materials Part 1: Designation system and basis for specifications DIN ISO 976, Rubber and plastics Polymer dispersions and rubber latices Determination of pH DIN ISO 8130-
7、1, Coating powders Part 1: Determination of particle size distribution by sieving EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15023-2April 2006ICS 83.080.20English VersionPlastics - Poly(vinyl alcohol) (PVAL) materials - Part 2:Determination of properties (ISO 15023-2:2003)Plastiques - Mat
8、riaux en poly(alcool de vinyle) (PVAL) -Partie 2: Dtermination des proprits (ISO 15023-2:2003)Kunststoffe - Polyvinylalkohol (PVAL)-Formmassen - Teil 2:Bestimmung von Eigenschaften (ISO 15023-2:2003)This European Standard was approved by CEN on 16 March 2006.CEN members are bound to comply with the
9、CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to
10、 any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CE
11、N members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switze
12、rland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN IS
13、O 15023-2:2006: EEN ISO 15023-2:2006 (E) 2 Foreword The text of ISO 15023-2:2003 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15023-2:2006 by Technical Committee CEN/TC 249 “Plastics”, the
14、secretariat of which is held by IBN. 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 October 2006, and conflicting national standards shall be withdrawn at the latest by October 2006. According to
15、 the CEN/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, Lux
16、embourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 15023-2:2003 has been approved by CEN as EN ISO 15023-2:2006 without any modifications. Contents Page Foreword2 1 Scope 3 2 Normative
17、references 3 3 Determination of properties4 Annex A (normative) Determination of volatile-matter content .5 Annex B (normative) Determination of sodium acetate content7 Annex C (normative) Calculation of ash.10 Annex D (normative) Determination of degree of hydrolysis.11 Annex E (normative) Determin
18、ation of viscosity of 4 % aqueous solution by the Brookfield Test method or the inclined-tube falling-ball method 14 EN ISO 15023-2:2006 (E) 3 1 Scope This part of ISO 15023 specifies the methods to be used in determining the properties of poly(vinyl alcohol), which is normally prepared by hydrolysi
19、s of poly(vinyl acetate) and whose composition comprises vinyl alcohol monomeric units and vinyl acetate monomeric units. This part of ISO 15023 is applicable to poly(vinyl alcohol) with a vinyl alcohol unit content (degree of hydrolysis) from 70 mol % to 100 mol %. In addition to the designatory pr
20、operties specified in ISO 15023-1 (degree of hydrolysis and viscosity of an aqueous solution), this part of ISO 15023 includes a number of other properties which are commonly used to specify PVAL materials (see Table 1). 2 Normative references The following referenced documents are indispensable for
21、 the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 976:1996, Rubber and plastics Polymer dispersions and rubber latices Determination of pH ISO 6587:199
22、2, Paper, board and pulps Determination of conductivity of aqueous extracts ISO 8130-1:1992, Coating powders Part 1: Determination of particle size distribution by sieving ISO 12058-1:1997, Plastics Determination of viscosity using a falling-ball viscometer Part 1: Inclined-tube method ISO 15023-1:2
23、001, Plastics Poly(vinyl alcohol) (PVAL) materials Part 1: Designation system and basis for specifications EN ISO 15023-2:2006 (E) 4 3 Determination of properties In the determination of properties and the presentation of results, the standards, methods and special conditions listed in Table 1 shall
24、 apply. The properties listed in Table 1 are those appropriate to poly(vinyl alcohol). Table 1 Properties and test conditions Property Method Unit Test conditions and supplementary instructions Volatile-matter content Annex A % by mass 105 C, 3 h Sodium acetate content Annex B % by mass Titration or
25、 conductivity method Ash Annex C % by mass Degree of hydrolysis Annex D mol % Titration method Viscosity of 4 % aqueous solution Annex E mPas Rotational or inclined-tube falling-ball viscometer, 20 C Particle size distribution ISO 8130-1 % pH of aqueous solution ISO 976 Concentration (4,0 0,2) % EN
26、ISO 15023-2:2006 (E) 5 Annex A (normative) Determination of volatile-matter content A.1 Scope This annex specifies the method to be used for the determination of the volatile-matter content of PVAL. A.2 Principle The volatile-matter content is calculated from the loss in mass of a specimen heated at
27、 105 C for 3 h. A.3 Method A.3.1 Apparatus A.3.1.1 Constant-temperature oven, able to maintain a temperature of (105 2) C. A.3.1.2 Weighing dish, shallow, about 60 mm in diameter and 30 mm in height, of glass, aluminium or preferably stainless steel, with a lid. A.3.1.3 Balance, capable of weighing
28、to 0,001 g. A.3.1.4 Desiccator, containing silica gel as a drying agent. A.3.2 Procedure Carry out the determination in duplicate. Weigh the dish (A.3.1.2) with its lid to the nearest 0,001 g (m0), after heating it in the oven (A.3.1.1) maintained at (105 2) C for 1 h and cooling it to room temperat
29、ure in the desiccator (A.3.1.4). Spread about 5 g of resin evenly over the bottom of the dish, replace the lid and weigh to the nearest 0,001 g (m1). Place the assembly in the oven at (105 2) C, remove the lid (leaving it in the oven) and close the oven door. After 3 h 5 min, remove the assembly fro
30、m the oven, allow to cool in the desiccator and weigh to the nearest 0,001 g (m2). A.4 Expression of results Calculate the volatile-matter content wVM, as a percentage by mass, from the following equation: 12VM10100mmwmm=where m0is the mass, in g, of the dish; m1is the initial mass, in g, of the dis
31、h plus test portion; EN ISO 15023-2:2006 (E) 6 m2is the mass, in g, of the dish plus test portion after heating. Calculate the mean of the results of the two determinations and express the final result to two places of decimals. A.5 Test report The test report shall include the following particulars
32、: a) a reference to this part of ISO 15023; b) all details necessary for complete identification of the material tested; c) the volatile-matter content, calculated as the arithmetic mean of the two determinations; d) the individual results of the two determinations; e) the date of the test. EN ISO 1
33、5023-2:2006 (E) 7 Annex B (normative) Determination of sodium acetate content B.1 Scope This annex specifies the method to be used for the determination of the sodium acetate content of PVAL. The content can be determined either by a titration method or by a conductivity method. Additives can interf
34、ere with the determination, and these methods may not be suitable for PVAL containing them. B.2 Principle B.2.1 Titration method The sample is dissolved in water and the solution titrated with hydrochloric acid using methyl orange as indicator. The sodium acetate content is calculated as a percentag
35、e by mass. B.2.2 Conductivity method The conductivity of an aqueous solution of the sample is measured in a conductometer. The sodium acetate content of the solution is determined by calibrating the conductometer with solutions containing known amounts of sodium acetate. B.3 Titration method B.3.1 R
36、eagents B.3.1.1 Hydrochloric acid, 0,1 mol/l. B.3.1.2 Methyl orange indicator, 1 g/l solution in ethanol, or mixed methylene blue/methyl yellow indicator, prepared by mixing equal parts of a 0,1 % solution of methylene blue in reagent-grade ethanol with a 0,1 % solution of methyl yellow in reagent-g
37、rade ethanol. B.3.2 Apparatus B.3.2.1 Conical flask, 300 ml, with ground-glass stopper. B.3.2.2 Cylinder, 200 ml, graduated in 2 ml. B.3.2.3 Burette, 50 ml, graduated in 0,1 ml. B.3.3 Procedure Carry out the determination in duplicate. Weigh about 5 g of sample to the nearest 0,001 g into the conica
38、l flask (B.3.2.1), add about 150 ml of water and dissolve by heating. EN ISO 15023-2:2006 (E) 8 A sample with a low degree of hydrolysis may sometimes cause the solution to become turbid. If this occurs, cool the solution slowly while stirring gently. Alternatively, a 3:1 water/methanol mixture may
39、be used. After dissolution, cool and titrate with 0,1 mol/l hydrochloric acid to an end point where the solution turns from orange-yellow to red if methyl orange is used as indicator or from green to light purple if methylene blue/methyl yellow is used. Carry out a blank test separately. B.3.4 Expre
40、ssion of results Calculate the sodium acetate content wNaAc, as a percentage by mass, from the following equation: 10NaAc( ) 0,082 03100VV cwm= where V1is the volume, in ml, of hydrochloric acid required for the test solution; V0is the volume, in ml, of hydrochloric acid required for the blank; c is
41、 the actual concentration, in mol/l, of the hydrochloric acid; 0,082 03 is the molecular mass of sodium acetate divided by 1 000; m is the mass, in g, of the test portion. Calculate the mean of the results of the two determinations and express the final result to two places of decimals. B.4 Conducti
42、vity method B.4.1 Reagent B.4.1.1 Sodium acetate, reagent grade. B.4.2 Apparatus B.4.2.1 Conical flask, 100 ml, with ground-glass stopper. B.4.2.2 Cylinder, 100 ml, graduated in 1 ml. B.4.2.3 Conductivity meter, as specified in ISO 6587. B.4.2.4 Thermometer, graduated in 0,1 C. B.4.2.5 Volumetric fl
43、ask, 100 ml, with ground-glass stopper. B.4.3 Procedure Carry out the determination in duplicate. Weigh 0,5 g of sample to the nearest 0,001 g into a conical flask, add about 50 ml of water and dissolve by heating. A sample with a low degree of hydrolysis may sometimes cause the solution to become t
44、urbid. If this occurs, cool the solution slowly while stirring gently. EN ISO 15023-2:2006 (E) 9 Transfer the solution to a 100 ml volumetric flask and make up to the mark with water. Transfer about 50 ml of the aqueous solution in the volumetric flask to the measuring cell of the conductivity meter
45、. Measure the conductivity at 30 C 0,1 C. B.4.4 Calibration curve Prepare the calibration curve as follows: Prepare four or five aqueous sodium acetate solutions covering a suitable range of concentrations and measure their conductivities. Prepare the calibration curve by plotting the conductivity v
46、alues against the corresponding sodium acetate concentrations (g/100 ml). B.4.5 Expression of results Calculate the sodium acetate content wNaAc, as a percentage by mass, from the following equation: NaAcNaAc100wm= where NaAcis the concentration of sodium acetate in the test solution, in g/100 ml, o
47、btained from the calibration curve; m is the mass, in g, of the test portion. Calculate the mean of the results of the two determinations and express the final result to two places of decimals. B.5 Test report The test report shall include the following particulars: a) a reference to this part of IS
48、O 15023; b) all details necessary for complete identification of the material tested; c) the sodium acetate content, calculated as the arithmetic mean of the two determinations; d) the individual results of the two determinations; e) the date of the test. EN ISO 15023-2:2006 (E) 10 Annex C (normativ
49、e) Calculation of ash C.1 Scope This annex specifies the method to be used for the calculation of the ash of PVAL. C.2 Principle The ash expressed as sodium oxide is calculated from the sodium acetate content determined in Annex B. C.3 Calculation From each of the sodium acetate contents determined in Annex B, calculate the ash wAsh, as a percentage by mass, from the following equation: Ash NaAc0,378ww= where wNaAcis the sodium acetate content, in %; 0,378 is a factor for converting the mass of sodium a
