BS EN ISO 4625-2-2005 Binders for paint and varnishes - Determination of softening point - Cup-and-ball method《涂料和清漆用粘合剂 软化点的测定 环-球接合法》.pdf

1、BRITISH STANDARDBS EN ISO 4625-2:2006Incorporating Amendment No. 1 (to renumber BS ISO 4625-2:2004 as BS EN ISO 4625-2:2006)Binders for paints and varnishes Determination of softening point Part 2: Cup-and-ball methodThis European Standard EN ISO 4625-2:2006 has the status of a British StandardICS 8

2、7.060.20BS EN ISO 4625-2:2006This British Standard was published under the authority of the Standards Policy andStrategy Committee on 2 February 2005 BSI 2006ISBN 0 580 45383 9National forewordThis British Standard is the official English language version of EN ISO 4625-2:2006. It is identical with

3、ISO 4625-2:2004.The UK participation in its preparation was entrusted to Technical CommitteeSTI/3, Paints, 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-referencesThe British Standar

4、ds which implement international 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

5、 not purport to 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 immunityfrom legal obligations. aid enquirers to understand the text; present to the responsible international/European

6、committee anyenquiries on the interpretation, or proposals for change, and keep theUK interests informed; monitor related international and European developments andpromulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN ISOtitle page, Foreword

7、page, the ISO title page, pages ii to iv, pages 1 to 6,an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when thedocument was last issued.Amendments issued since publicationAmd. No. Date Comments16195 July 2006 Renumbers BS ISO 4625-2:2004 as BS EN I

8、SO 4625-2:2006EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 4625-2February 2006ICS 87.060.20English VersionBinders for paints and varnishes - Determination of softeningpoint - Part 2: Cup-and-ball method (ISO 4625-2:2004)Liants pour peintures et vernis - Dtermination du point deramollissemen

9、t - Partie 2: Mthode de la coupe et de labille (ISO 4625-2:2004)Bindemittel fr Beschichtungsstoffe - Bestimmung derErweichungstemperatur - Teil 2: Verfahren mit Becher undKugel (ISO 4625-2:2004)This European Standard was approved by CEN on 16 January 2006.CEN members are bound to comply with the CEN

10、/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 an

11、y 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.CEN m

12、embers 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, Switzerla

13、nd 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 ISO 4

14、625-2:2006: EEN ISO 4625-2:2006 (E) Foreword The text of ISO 4625-2:2004 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 4625-2:2006 by Technical Committee CEN/TC 139 “Paints and v

15、arnishes“, the secretariat 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 August 2006, and conflicting national standards shall be withdrawn at the latest by August 2006.

16、 According to 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, L

17、ithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement noticeThe text of ISO 4625-2:2004 has been approved by CEN as EN ISO 4625-2:2006 without any modifications. Reference numberISO 4625-2:2004(E)IN

18、TERNATIONALADNATSDRISO4-5262tide tsriFino-400251-80Binders for paints and varnishes Determination of softening point Part 2: Cup-and-ball method Liants pour peintures et vernis Dtermination du point de ramollissement Partie 2: Mthode de la coupe et de la bille INTERNATIONALSTANDARDISO4625-2First edi

19、tion2004-08-15EN ISO 46252:2006ivEN ISO 46252:20066vContents PageForeword vi1 Scope 12 Normative references . 13 Terms and definitions. 14 Principle . 15 Apparatus. 26 Calibration of apparatus using a primary standard 37 Instrument check of apparatus using a secondary standard. 38 Filling the cups w

20、ith resin 49 Procedure. 510 Expression of results 511 Precision and bias 512 Test report 6EN ISO 46252:2006viForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is

21、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 non-governmental, in liaison with ISO, also take part

22、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, Part 2. The main task of technical committees is to pre

23、pare International Standards. 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

24、some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 4625-2 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 10, Test methods for binders for paints and varn

25、ishes, in collaboration with ASTM D01.34, Naval Stores. It has been harmonized with ASTM D 6090-99, Standard Test Method for Softening Point of Resins (Mettler Cup and Ball Method).ISO 4625 consists of the following parts, under the general title Binders for paints and varnishes Determination of sof

26、tening point: Part 1: Ring-and-ball method Part 2: Cup-and-ball methodEN ISO 46252:2006INTENRATIONAL TSANDADR IS-5264 O2:(4002E)1Binders for paints and varnishes Determination of softening point Part 2: Cup-and-ball method 1 Scope This part of ISO 4625 specifies a method for determining the softenin

27、g point of resins (including rosin) by means of a cup-and-ball apparatus and can, under user-defined conditions, give results comparable to those obtained using the ring-and-ball method (ISO 4625-1). 2 Normative references The following referenced documents are indispensable for the application of t

28、his document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 4625-1, Binders for paints and varnishes Determination of softening point Part 1: Ring-and-ball methodISO 5725-1, Accuracy

29、 (trueness and precision) of measurement methods and results Part 1: General principles and definitions3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1softening point temperature at which a test sample in a cylindrical cup with a 6,35 mm hole

30、in the bottom, with a stainless-steel ball 8,7 mm in diameter centred on top of the test sample in the cup, flows downward a distance of 19 mm to interrupt a light beam as the test sample is heated at a constant rate in air 4 Principle In general, with materials of the types mentioned in Clause 1, s

31、oftening does not take place at a definite temperature. As the temperature rises, these materials gradually change from brittle or exceedingly thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed, close

32、ly defined method if the results obtained are to be comparable. A test sample, with the ball on it, is placed in a cup and heated at a specified rate. The softening test sample is forced downwards by the weight of the ball. The temperature at which the test sample has sunk by 19 mm is called the sof

33、tening point. EN ISO 46252:200625 Apparatus 5.1 Softening point apparatus1), consisting of a control unit with a digital temperature indicator, matched measuring cell, cartridge assembly (cup and upper portion) and accessories. The control unit automatically regulates the heating rate of the measuri

34、ng cell. The softening point is indicated on the readout, and the heating programme is stopped, when the test sample flow triggers a photocell detector. Further details are given in 5.1.1 to 5.1.4. 5.1.1 Central processor, capable of regulating the heating rate to provide a continuous, linear increa

35、se in temperature from 25 C to 375 C. 5.1.2 Measuring cell, capable of heating the cup assembly (5.4) at a constant rate with an accuracy of r 0,2 C/min. It shall include a sensing system capable of detecting the softening point with a precision of 0,1 C. 5.1.3 Cup assembly, made of chromium-plated

36、brass, consisting of the cup itself and an upper portion, conforming to the dimensions shown in Figure 1. 5.1.4 Ball, made of stainless steel, 8,7 mm in diameter and weighing (2,77 r 0,22) g. Dimensions in millimetres Figure 1 Cup 1) The apparatus is available commercially. Details may be obtained f

37、rom the Secretariat of ISO/TC 35/SC 10. EN ISO 46252:200636 Calibration of apparatus using a primary standard6.1 General This step, required only occasionally, is designed to establish that the temperature indicated by the instrument is in agreement with a known standard. A special cup with a bottom

38、 orifice of 2,8 mm is used instead of the one specified for testing the resin. NOTE The stainless-steel ball is not used during calibration. 6.2 ReagentUse either analytical reagent or primary standard grade benzoic acid for the calibration. As this material is hygroscopic, store it in a tightly sea

39、led container and replace it with fresh material from a newly opened supply if the softening point of the material is out of the expected range. 6.3 Procedure 6.3.1 Filling the cup Place the cup on a clean, flat surface and fill it with benzoic acid crystals. Hand press the material into the cup wit

40、h a 9,2 mm rod of dowel stock or equivalent. Refill and repeat the compression step until the cup is filled with benzoic acid. Remove any crystals from the exterior of the cup. 6.3.2 Heating Preheat the measuring cell to 121 C, and maintain it at that temperature. Place the cartridge assembly contai

41、ning the benzoic acid in position in the measuring cell, taking care that the slits for the light beam are properly positioned. With the instrument set in the dropping-point mode, start the required method, which includes a waiting period of 30 s to allow temperature equilibration between the measur

42、ing cell and benzoic acid followed by an automatic temperature ramp of 0,2 C/min. The temperature will rise steadily at the correct rate until the drop point is reached, then remain steady on the readout. 6.3.3 Cleaning Immediately remove the cartridge assembly. Check to determine that benzoic acid

43、has passed through the light beam and no pre-triggering has occurred. If a malfunction is suspected, repeat the entire procedure. Inspect the apparatus carefully to ensure that no residue remains. Wash the cartridge parts with a suitable solvent to remove last traces of residue. 6.3.4 Interpretation

44、 If the result is not (123,5 r 0,5) C, repeat the determination. If the second value remains outside the acceptable range, repeat the determination using a fresh cup-full of benzoic acid. If the results remain outside the acceptable range, the instrument requires recalibration or repair. Consult the

45、 manufacturers instruction manual. 7 Instrument check of apparatus using a secondary standardThe primary calibration standard, benzoic acid, might not have a dropping point similar to the softening point of the resin being tested. In such cases, it is desirable to calibrate the instrument using a se

46、condary standard having a dropping point similar to that of the resin being tested. Materials suitable for use as secondary standards are listed, but are not limited to, those in Table 1. Demonstration of conformance to the dropping point of benzoic acid shall be completed before a secondary standar

47、d is used. EN ISO 46252:20064Table 1 Materials suitable as secondary standards for cup-and-ball softening point Approximate dropping point CMaterial 60 Stearyl alcohol 80 Diphenyl carbonate 100 Phenoxyacetic acid 4-tert-Butylphenol Methyl urea 110 m-Toluic acid Resorcinol 120 Benzoic acid 130 Methyl

48、 4-hydroxybenzoate Urea Benzamide 1,10-Decanedicarboxylic acid 140 Dimethyl terephthalate o-Toluamide Follow the same procedure as in 6.3.2 and 6.3.3 but start about 3 C below the actual dropping point of the secondary standard. 8 Filling the cups with resin 8.1 Preparation Fold the tab on an oil-fr

49、ee disposable aluminium weighing dish to a horizontal position and pinch a pour spout into the dish directly opposite the tab. Weigh 5 g to 10 g of resin into the dish. Place the dish and resin on a preheated hot-plate, and cover with a 600 ml or larger beaker. Heat the resin until it is almost melted. Remove the beaker from the hot-plate, grasp the tab with forceps or needle-nose pliers, and stir the resin with a probe-type thermometer until it is completely melted and homogeneous. Avoid entraining air in the resin melt. The te