1、February 2011 Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC
2、S 87.060.20!$my“1748604www.din.deDDIN EN ISO 14446Binders for paints and varnishes Determination of the viscosity of industrial cellulose nitrate solutionsand classification of such solutions (ISO 14446:1999)English translation of DIN EN ISO 14446:2011-02Bindemittel fr Beschichtungsstoffe Bestimmung
3、 der Viskositt technischer Cellulosenitrat-Lsungen und Einteilung solcherLsungen (ISO 14446:1999)Englische bersetzung von DIN EN ISO 14446:2011-02Liants pour peintures et vernis Dtermination de la viscosit des solutions de nitrate de cellulose industrielles etclassification de ces solutions (ISO 144
4、46:1999)Traduction anglaise de DIN EN ISO 14446:2011-02SupersedesDIN ISO 14446:2002-04www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1102.11 DIN EN ISO 14446:2011-02 2 A comma is used as the decimal marker. National foreword This
5、standard has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes”, Subcommittee SC 10 “Test methods for binders for paints and varnishes” (Secretariat: DIN, Germany) in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). The responsi
6、ble German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee), Working Committee NA 002-00-02 AA Lackrohstoffe. The DIN Standards corresponding to the International Standards referred to in this documen
7、t are as follows: ISO 2811-1 DIN EN ISO 2811-1 ISO 2811-2 DIN EN ISO 2811-2 ISO 2811-3 DIN EN ISO 2811-3 ISO 12058-1 DIN EN ISO 12058-1 ISO 15528 DIN EN ISO 15528 Amendments This standard differs from DIN ISO 14446:2002-04 as follows: a) the status of the standard has been changed to that of a Europ
8、ean Standard; b) normative references have been updated; c) the standard has been editorially revised. Previous editions DIN 53179: 1965-03, 1970-06, 1979-02 DIN ISO 14446: 2002-04 National Annex NA (informative) Bibliography DIN EN ISO 2811-1, Paints and varnishes Determination of density Part 1: P
9、yknometer method DIN EN ISO 2811-2, Paints and varnishes Determination of density Part 2: Immersed body (plummet) method DIN EN ISO 2811-3, Paints and varnishes Determination of density Part 3: Oscillation method DIN EN ISO 12058-1, Plastics Determination of viscosity using a falling-ball viscometer
10、 Part 1: Inclined-tube method DIN EN ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14446 November 2010 ICS 87.060.20; 83.080.20 English Version Binders for paints and varnishes - Determination of the viscosit
11、y of industrial cellulose nitrate solutions and classification of such solutions (ISO 14446:1999) Liants pour peintures et vernis - Dtermination de la viscosit des solutions de nitrate de cellulose industrielles et classification de ces solutions (ISO 14446:1999) Bindemittel fr Beschichtungsstoffe -
12、 Bestimmung der Viskositt technischer Cellulosenitrat-Lsungen und Einteilung solcher Lsungen (ISO 14446:1999) This European Standard was approved by CEN on 16 October 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europe
13、an 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 CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English
14、, 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 CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, C
15、roatia, 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, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDA
16、RDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14446:2010: EContents DIN EN ISO 14446:2011-02 EN
17、 ISO 14446:2010 (E) 2 Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Apparatus and reagents5 5 Sampling and preparation of samples for testing5 6 Preparation of apparatus for testing5 7 Procedure .6 8 Expression of results 6 9 Precision.6 9.1 Repeatability (r) .6 9.2 Reproducibilit
18、y (R) .7 10 Test report 7 Annex A (normative) Classification system for industrial cellulose nitrate .8 Foreword The text of ISO 14446:1999 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
19、 EN ISO 14446:2010 by Technical Committee CEN/TC 139 “Paints and varnishes” 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 May 2011, and conflicting natio
20、nal standards shall be withdrawn at the latest by May 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENEL
21、EC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania
22、, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 14446:1999 has been approved by CEN as a EN ISO 14446:2010 without any modification. DIN EN ISO 14446:2011-02 EN ISO 14446:20
23、10 (E) 3 1 ScopeThis International Standard specifies a method of determining the viscosity of industrial cellulose nitrate, usuallyreferred to as nitrocellulose, the nitrogen content of which can vary between 10,7 % by mass and 12,6 % by mass,depending on the type.It also gives a classification sys
24、tem for industrial cellulose nitrate solutions (see annex A) which is based onviscosity measurements made using the method. The use of a standard procedure results in “standard“ types andavoids classification differences which could be caused by the fact that there are many ways of determiningviscos
25、ity and a wide variety of solvents available.2 Normative referencesThe following normative documents contain provisions which, through reference in this text, constitute provisions ofthis International Standard. For dated references, subsequent amendments to, or revisions of, any of thesepublication
26、s do not apply. However, parties to agreements based on this International Standard are encouraged toinvestigate the possibility of applying the most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative document referred to applies. M
27、embers of ISO and IECmaintain registers of currently valid International Standards.ISO 760:1978, Determination of water Karl Fischer method (General method).ISO 2811-1:1997, Paints and varnishes Determination of density Part 1: Pyknometer method.ISO 2811-2:1997, Paints and varnishes Determination of
28、 density Part 2: Immersed body (plummet) method.ISO 2811-3:1997, Paints and varnishes Determination of density Part 3: Oscillation method.ISO 12058-1:1997, Plastics Determination of viscosity using a falling-ball viscometer Part 1: Inclined-tubemethod.ISO 15528:1), Paints and varnishes Sampling.3 Pr
29、incipleThe cellulose nitrate is dissolved in an acetone/water mixture at a concentration which will depend on the type ofcellulose nitrate concerned. The density of the solution is determined using a pyknometer and the viscosity using aHppler falling-ball viscometer. The dynamic viscosity of the sol
30、ution is calculated from the results obtained.1)To be published. (Revision of ISO 842:1984 and ISO 1512:1991)DIN EN ISO 14446:2011-02 EN ISO 14446:2010 (E) 4 4 Apparatus and reagentsOrdinary laboratory apparatus and glassware, together with the following:4.1 Falling-ball viscometer, as specified in
31、ISO 12058-1, using ball No. 4.4.2 Thermostat, capable of maintaining the water jacket round the falling-ball viscometer at (20 0,1) C.4.3 Stopwatch, accurate to 0,1 s.4.4 Drying oven, capable of being maintained at (65 2) C, with a back-up safety system to ensure that thistemperature is not exceeded
32、.4.5 Analytical balance, capable of weighing to 1 mg.4.6 Bottle-shaking or rolling device.4.7 Pyknometer, capacity 25 ml, as specified in ISO 2811-1, or plummet, as specified in ISO 2811-2, oroscillator, as specified in ISO 2811-3.4.8 Weighing bottle, capacity 250 ml, with a wide mouth and stopper.4
33、.9 Watch glass or Petri dish.4.10 Acetone/water mixture, containing (5 0,2) % by mass of water. The water content of the mixture shall bechecked using the method described in ISO 760.5 Sampling and preparation of samples for testingWARNING For safety reasons, cellulose nitrate should always be moist
34、ened with water or a suitableorganic liquid, normally ethanol, isopropanol or butanol.5.1 Take a representative sample of the cellulose nitrate to be tested, as described in ISO 15528.5.2 Spread the moist sample in a thin layer on a watch glass or Petri dish and heat it in an air oven at (65 2) Cto
35、constant mass. This is reached when the results of two weighings made at an interval of 30 min do not differ bymore than 1 mg.For safety reasons, the door of the oven shall be left slightly open.5.3 Allow the dried cellulose nitrate to cool in a desiccator and keep it in the desiccator until needed
36、for weighingout the test portion.NOTE Cellulose nitrate is hygroscopic.Do not store dried cellulose nitrate. Any dried cellulose nitrate not used shall be moistened again.6 Preparation of apparatus for testing6.1 Clean the viscometer, the pyknometer or plummet or oscillator and the weighing bottle w
37、ith acetone before useand dry in a stream of clean, dry air.Repeat this cleaning procedure before every determination.6.2 Determine the viscometer constant K (see ISO 12058-1) at a temperature of (20 0,1) C with a certifiedreference liquid. Repeat this determination from time to time.DIN EN ISO 1444
38、6:2011-02 EN ISO 14446:2010 (E) 5 7 Procedure7.1 Weigh into the weighing bottle, to the nearest 1 mg, an amount of the dried cellulose nitrate sufficient for thedetermination of the dynamic viscosity and the density. If the type of cellulose nitrate in the sample is known, addthe quantity of acetone
39、 necessary to give the concentration required for that particular type of cellulose nitrate (seeTable A.1) and stopper the bottle. If the type of cellulose nitrate is not known, make an educated guess as to theamount of acetone necessary.7.2 Shake or roll the bottle for 6 h at a temperature of (20 5
40、) C to dissolve the cellulose nitrate. If the cellulosenitrate is not completely dissolved after this time, discard the solution.7.3 Determine immediately, to the nearest 0,1 s, the time of fall using the falling-ball viscometer method describedin ISO 12058-1 four times at a temperature of (20 0,1)
41、C using ball No. 4.The times of fall shall not differ by more than 0,5 s.7.4 Determine from another portion of the test solution the density with a pyknometer, using the method describedin ISO 2811-1, or a plummet, using the method described in ISO 2811-2, or an oscillator, using the methoddescribed
42、 in ISO 2811-3.7.5 If the type of cellulose nitrate in the sample is not known, carry out two further determinations using testsolutions of concentrations which will give viscosities successively closer to (400 25) mPa s.8 Expression of results8.1 The dynamic viscosity h, in mPa s, is given by the f
43、ollowing equation:hrr=-Kt()12whereK is the viscometer constant, in mPa s cm3/(g s) (see ISO 12058-1:1997, Table 1);r1is the density, in g/cm3, of the ball;r2is the density, in g/cm3, of the cellulose nitrate solution;t is the time of fall, in s, of the ball.8.2 To determine the type of cellulose nit
44、rate in a sample in which the type is not known, plot a curve ofconcentration versus viscosity for the three determinations carried out (see 7.5) and read off the concentration ofthe solution having a viscosity of (400 25) mPa s. Knowledge of the N2content will enable the designation to beread from
45、Table A.1.9 PrecisionThe following precision data have been taken from ISO 12058-1.9.1 Repeatability (r)The value below which the absolute difference between two single test results, each the mean of duplicates,obtained on identical material by one operator in one laboratory within a short interval
46、of time using the standardizedtest method, may be expected to lie with a 95 % probability is 0,5 %.DIN EN ISO 14446:2011-02 EN ISO 14446:2010 (E) 6 9.2 Reproducibility (R)The value below which the absolute difference between two test results, each the mean of duplicates, obtained onidentical materia
47、l by operators in different laboratories using the standardized test method, may be expected to liewith a 95 % probability is 2 %.10 Test reportThe test report shall contain at least the following information:a) all details necessary to identify the product tested;b) a reference to this Internationa
48、l Standard (ISO 14446);c) the concentration of cellulose nitrate in the test solution, in % by mass;d) the result of the test, as indicated in clause 8;e) details of any incident which may have affected the result;f) any deviation from the test method specified;g) the date of the test.DIN EN ISO 144
49、46:2011-02 EN ISO 14446:2010 (E) 7 Annex A(normative)Classification system for industrial cellulose nitrateThe classification system for industrial cellulose nitrate comprises two elements (see Table A.1):a number indicating the concentration of the solution that is required to give a viscosity of (400 25) mPa s,followed bya letter identifying the solvent in which it is soluble (corresponding to the N2content), i.e.E in the case of an ester-soluble grade (N2content ab
