1、BRITISH STANDARD BS EN ISO 4608:1998 BS 2782-4: Method 454E: 1998 Plastics Homopolymer and copolymer resins of vinyl chloride for general use Determination of plasticizer absorption at room temperature The European Standard EN ISO 4608:1998 has the status of a British Standard ICS 83.080.20BSENISO46
2、08:1998 This British Standard, having been prepared under the directionof the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 July 1998 BSI 04-1999 ISBN 0 580 29861 2 National foreword This British Standard is the English
3、 language version of EN ISO4608:1998. It is identical with ISO 4608:1998. It supersedes BS 2782-4:Method 454E:1992 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/34, Vinyl materials, which has the responsibility to: aid enquirers to understand th
4、e 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 international and European developments and promulgate them in the UK. A list of organizations represented on this com
5、mittee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC standards normally include an annex which lists normative references to international publications with their corresponding European publications. The BritishStandards which imple
6、ment 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 BSI Standards Electronic Catalogue. A British Standard does not purpo
7、rt 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. Summary of pages This document comprises a front cover, an inside front co
8、ver, pages i and ii, the EN ISO title page, page 2, the ISO title page, page ii, pages 1 to 4 and aback cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued sinc
9、e publication Amd. No. Date CommentsBSENISO4608:1998 BSI 04-1999 i Contents Page National foreword Inside front cover Foreword 2 Foreword ii Text of EN ISO 4608 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4608 May 1998 ICS 83.080.20 Descriptors: See ISO document English version
10、 Plastics Homopolymer and copolymer resins of vinyl chloride for general use Determination of plasticizer absorption at room temperature (ISO 4608:1998) Plastiques Rsines dhomopolymres et de copolymres de chlorure de vinyle usages gnraux Dtermination de la prise de plastifiant temprature ambiante (I
11、SO 4608:1998) Kunststoffe Vinylchlorid(VC) Homopolymere und Copolymere fr allgemeine Anwendungen Bestimmung der Weichmacheraufnahme bei Raumtemperatur (ISO 4608:1998) This European Standard was approved by CEN on 9 April 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations
12、 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 Secretariat or to any CEN member. This European
13、 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 official versions. CEN members are the national
14、 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 Standardization Comit Europen de Normalisation Europisches K
15、omitee 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 4608:1998 EENISO4608:1998 BSI 04-1999 2 Foreword The text of the International Standard ISO4608:1998
16、 has been prepared by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee CEN/TC 249 “Plastics”, the 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 endorseme
17、nt, at the latest by November 1998, and conflicting national standards shall be withdrawn at the latest by November 1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium
18、, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. NOTE FROM CEN/CS: The foreword is susceptible to be anmended on reception of the German language version. The confirmed
19、or amended foreword, and when appropriate, the normative Annex ZA for the references to international publications with their relevant European publications will be circulated with the German version. Endorsement notice The text of the International Standard ISO4608:1998 was approved by CEN as a Eur
20、opean Standard without any modification. Contents Page Foreword 2 1 Scope 1 2 Normative reference 1 3 Principle 1 4 Apparatus and materials 1 5 Procedure 1 6 Expression of results 2 7 Precision 2 8 Test report 2 Figure 1 Example of centrifuge tube (without sieve plate) and sheath 3 Figure 2 Example
21、of centrifuge tube (with sieve plate) and sheath 4 Table 1 Precision data 2ENISO4608:1998 ii BSI 04-1999 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 norm
22、ally 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 non-governmental, in liaison with ISO, also take part in t
23、he work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard re
24、quires approval by at least 75% of the member bodies casting a vote. International Standard ISO 4608 was prepared by Technical Committee ISO/TC61, Plastics, Subcommittee SC 9, Thermoplastic materials. This third edition cancels and replaces the second edition (ISO4608:1984), which has been technical
25、ly revised. Descriptors: Plastics, vinyl resins, polyvinyl chloride, tests, determination, plasticizer absorption.ENISO4608:1998 BSI 04-1999 1 1 Scope This International Standard specifies a method for determining plasticizer absorption at room temperature. It is applicable to PVC general- purpose r
26、esins and filler resins (designated “G” and “F” in ISO1060-1:1998, Plastics Homopolymer and copolymer resins of vinyl chloride Part 1: Designation system and basis for specifications). The object of the test is to determine the quantity of plasticizer absorbed by a resin at room temperature to give
27、a dry mixture. The results give a general indication of the plasticizer absorption of a resin at room temperature. They indicate the usefulness of resins for the manufacture of plasticized dry blends, particularly when taken in conjunction with the results of plasticizer absorption tests under hot c
28、onditions. 2 Normative reference The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based
29、 on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 1385-1:1977, Phthalate esters for industrial use Methods of tes
30、t Part 1: General. 3 Principle An excess of bis-(2-ethylhexyl) phthalate (DOP) is added to a specified amount of resin. The mixture is then centrifuged under defined conditions and the amount of plasticizer retained by the resin determined. 4 Apparatus and materials Ordinary laboratory apparatus, pl
31、us the following: 4.1 Balance, capable of weighing to 0,1mg. 4.2 Burette, for example 50 cm 3 , graduated at 0,1 cm 3intervals. 4.3 Centrifuge, whose rotor turns in a horizontal plane and which has an acceleration under the test conditions of 24500 ms 2to 29500 ms 2measured at the bottoms of.the tub
32、es, with, if necessary, a cooling system to prevent the temperature of the mixture from exceeding 30 C at the end of centrifuging for 60 min. NOTEIt is permissible to use different centrifuging conditions,i.e. a different acceleration, a different time and smaller centrifuge tubes (see 4.4), provide
33、d that it has been verified that the results obtained are equivalent. 4.4 Centrifuge tubes, to fit the centrifuge used, each consisting either of a tube, made of glass or another material, with a conical bottom pierced by a hole of about 0,8mm diameter (see Figure 1) or of a cylindrical tube fitted
34、at one end with a sieve plate on which a filter paper can be placed (see Figure 2). The sieve plate is pierced by holes of diameter approximately 0,8mm. The holes are arranged concentrically approximately 4mm apart. 4.5 Sheaths, made of polyamide, polyethylene or any other suitable material, to fit
35、the centrifuge used, with a reduction tube at the bottom to support the centrifuge tube (see Figure 1 or Figure 2). 4.6 Cotton wool, pharmaceutical quality, having a DOP absorption measured under the test conditions (see 5.1) of approximately 10%, or, if a centrifuge tube with a sieve plate is used,
36、 filter paper, with a diameter is equal to the inner diameter of the centrifuge tube. NOTEAlternative materials to cotton wool may be used if it can be shown that they produce equivalent results, for example glass wool and PTFE-coated polyester felt. 4.7 Bis-(2-ethylhexyl) phthalate (DOP) When teste
37、d by the methods described in ISO1385-1 at 20 C, the DOP plasticizer used shall have the following properties: 5 Procedure 5.1 Measurement of DOP absorbed by the cotton wool or filter paper Following the procedure indicated in 5.2, carry out a blank test with a piece of cotton wool having a mass of
38、100mg 2mg or with a filter paper (if a centrifuge tube with a sieve plate is used), but without any resin. Determine the amount of DOP absorbed by the cotton wool or filter paper, in grams. 5.2 Determination Weigh a piece of cotton wool (100mg 2mg), place it in the centrifuge tube and pack it down s
39、lightly. When working with a centrifuge tube with a sieve plate, place a filter paper on the sieve plate. Weigh the tube and cotton wool or filter paper to the nearest 0,1mg. Weigh directly into the tube 2,000g 0,001g, to the nearest 0,1mg, of the resin under test. Density 0,982 g/cm 3to 0,984 g/cm
40、3 Refractive index 1,486 to 1,487 Dynamic viscosity 77 mPas to 83 mPasENISO4608:1998 2 BSI 04-1999 From the burette, run into the tube 4cm 3of DOP and allow it to stand for about 10min. NOTEIf smaller centrifuge tubes are used (see the note to 4.3), the following smaller quantities of material may b
41、e used: 1 g of resin under test; 2cm 3of DOP. Put the tube into its sheath and place the whole into one of the compartments of the centrifuge rotor (the other compartments being occupied by tubes containing other resin samples, all the tubes being balanced). Set the centrifuge to give an acceleratio
42、n of24500ms 2to 29500 ms 2at the bottoms of the tubes for60min. If necessary, switch on the cooling device during centrifuging. The temperature shall not exceed 30 C. Take the tube from its sheath, carefully wipe it to remove any DOP on the outside and weigh it to the nearest 0,1mg. 6 Expression of
43、results The room temperature plasticizer absorption, expressed as parts of DOP absorbed per 100 parts of resin (p.h.r.), is given by the formula where 7 Precision Interlaboratory trials conducted on three resins in five laboratories have shown that the repeatability standard deviation s r(within the
44、 same laboratory) and the reproducibility standard deviation s R(between different laboratories) depend on the plasticizer absorption, as shown inTable 1. Table 1 Precision data The centrifuge tubes and sheaths used (Figure 1 and Figure 2) have only a minor influence. 8 Test report The test report s
45、hall include the following information: a) a reference to this International Standard; b) all details necessary for identification of the sample tested; c) the centrifuging conditions (acceleration and time), if different from those specified in 5.2; d) the quantities of resin and DOP used, if diffe
46、rent from those specified in 5.2; e) the result of the test; f) the date of the test. m 0 is the mass, in grams, of DOP absorbed by the cotton wool or filter paper in the blank test (see 5.1); m 1 is the mass, in grams, of the centrifuge tube plus cotton wool or filter paper (see 5.2); m 2 is the ma
47、ss, in grams, of the centrifuge tube plus cotton wool or filter paper and resin sample (see 5.2); m 3 is the mass, in grams, of the centrifuge tube plus cotton wool or filter paper, resin and DOP absorbed, after centrifuging (see5.2). m 3 m 0 ()m 2 m 2 m 1 -100 Plasticizer absorption (%) approx. 5 a
48、pprox. 21 approx. 40 s r 0,25 0,37 0,42 s R 0,43 0,60 0,72ENISO4608:1998 BSI 04-1999 3 Figure 1 Example of centrifuge tube (without sieve plate) and sheathENISO4608:1998 4 BSI 04-1999 Figure 2 Example of centrifuge tube (with sieve plate) and sheath5 blankBS EN ISO 4608:1998 BS 2782-4: Method 454E:
49、1998 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments or editions. It is th
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