DIN 53177-2002 Binders for paints and varnishes - Measurement of the dynamic viscosity of liquid resins Resin solutions and oils by the capillary viscosimeter of isocelses type acc.pdf

1、ICS 87.060.20Bindemittel fr Beschichtungsstoffe Messung der dynamischenViskositt von flssigen Harzen, Harzlsungen und len mit demKapillarviskosimeter gleichschenkliger Bauart nach UbbelohdeIn keeping with current practice in standards published by the International Organization for Standardization(I

2、SO), a comma has been used throughout as the decimal marker.Ref. No. DIN 53177 : 2002-11English price group 06 Sales No. 010612.03DEUTSCHE NORM November 200253177Continued on pages 2 to 6. No part of this translation may be reproduced without the prior permission ofDIN Deutsches Institut fr Normung

3、e.V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).Determination of dynamic viscosity of liquidresins, resin solutions and oils using theUbbelohde capillary viscometerTranslation by DIN-Sprachendienst.In case of doubt, the German-

4、language original should be consulted as the authoritative text.ForewordThis standard has been prepared by Technical Committee Lackrohstoffe of the NormenausschussBeschichtungsstoffe und Beschichtungen (Paints and Varnishes Standards Committee).The capillary viscometers specified in DIN 51562-1 to D

5、IN 51562-3 for measuring kinematic viscosity haveproved satisfactory in practice, with a repeatability limit of 0,2 % if the Hagenbach correction is taken intoaccount. The measurement conditions specified in those standards have been included in this standard sothat viscometers having the same visco

6、meter constants are designated in the same way in both standards.The requirement for a somewhat more rugged viscometer for measuring the dynamic viscosity directlywithout determining the density is fulfilled by a viscometer having equal limbs, which was also developedby Ubbelohde. With a repeatabili

7、ty limit of 1 % (absolute), better information can be obtained with flow timesof around 100 s than with flow times using the ISO cup (cf. DIN EN ISO 2431), despite the omission of theHagenbach correction, which is below 5 % even with viscometer of size no. 1c.AmendmentsThis standard differs from the

8、 November 1990 edition in that it has been editorially revised and the normativereferences have been updated.Previous editionsDIN 53177: 1974-07, 1990-11.All dimensions are in millimetres.1 ScopeThe method described in this standard serves to determine the dynamic viscosity of liquid resins, resinso

9、lutions, oils and other liquids having Newtonian flow and used to produce paints and varnishes, impreg-nating resins, etc. The viscometers specified in this standard are intended for use for flow times of at least50 s and at temperatures ranging from 10 C to about 90 C, and are operated at measuring

10、 ranges extend-ing from 1,5 mPa. s to over 5 000 mPa. s, the upper limit being set by the onset of non-Newtonian flow,where viscosities of over 12 000 mPa. s are frequently encountered. In this context, reference is made toDIN 53012.SupersedesNovember 1990 edition.Page 2DIN 53177 : 2002-112 Normativ

11、e referencesThis standard incorporates, by dated or undated reference, provisions from other publications. These norma-tive references are cited at the appropriate places in the text, and the titles of the publications are listed below.For dated references, subsequent amendments to or revisions of a

12、ny of these publications apply to thisstandard only when incorporated in it by amendment or revision. For undated references, the latest edition ofthe publication referred to applies.DIN 1342-1 Viscosity Rheological conceptsDIN 51562-1 Determination of kinematic viscosity using the Ubbelohde viscome

13、ter Apparatus andmeasurement procedureDIN 51562-2 Determination of kinematic viscosity using the Ubbelohde microviscometerDIN 51562-3 Determination of kinematic viscosity using the Ubbelohde viscometer Relative incre-ment at short flow timesDIN 53012 Capillary viscometry of Newtonian liquids Sources

14、 of error and correctionsDIN EN ISO 2431 Determination of flow time of paints and varnishes by use of flow cups (ISO 2431 : 1993+ Corr 1 : 1994)DIN EN ISO 15528 Paints, varnishes and raw materials for paints and varnishes Sampling (ISO 15528 : 2000)ISO 719 : 1985 Glass Hydrolytic resistance of glass

15、 grains at 98 C Method of test and classificationDIN ISO 3310-1 Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth(ISO 3310-1 : 2000)3 ConceptsSee DIN 1342-1.4 PrincipleThe method is based on laminar flow of the test liquid through a capillary. Since the hydrostat

16、ic internal pressureis negligible during the measurement, the density of the test liquid is not involved and surface tension hasvirtually no effect, the method permits direct measurement of dynamic viscosity and requires the applicationof external pressure.5 Sampling and sample preparationA represen

17、tative sample of the test liquid sufficient for at least two measurements (about 20 ml for each test)shall be collected as described in DIN EN ISO 15528, removing suspended particles before measurement byfiltration or by sieving through an analytical sieve of aperture size 0,2 mm (as in DIN ISO 3310

18、-1).6 Number of measurementsViscosity shall be measured twice using a fresh sample each time.7 ApparatusThe following equipment shall be used.7.1 Ubbelohde capillary viscometer having two equal limbsThe viscometer (see figure 1) shall be made of glass and have a hydrolytic resistance corresponding t

19、o classHBG 1 as in ISO 719. Each limb shall have a bulb of equal volume at the same height1), one limb containing ameasuring capillary (sealed-in) with the viscometer constant permanently marked on it (the constant can alsobe determined in-house as described in subclause 8.3), the other limb having

20、permanent measuring marks (M1and M2).Since the diameter of the capillaries depends on the viscosity range required, several viscometers havingcapillaries of the same length (100 mm), but different internal capillary diameters, are used (see table 1 andfigure 1 for other dimensions).Calibrated precis

21、ion glass tubes shall be used for the capillaries. The volume of each of the two bulbs measuredbetween the marks shall be (7 t 0,5) ml. The limb above M2 may either be bent over about 50 mm below theend of the other limb, as shown in figure 1, or be straight and of the same length as the latter.1) T

22、he accuracy of the measurements is unaffected by whether the bulbs are spherical or somewhat elongatedat the tube attachment point, but it is important that their volumes are as equal as possible.Page 3DIN 53177 : 2002-11NOTE: The holder shown in figure 2 is suitable for suspending viscometers with

23、straight limbs in thermostats(see subclause 7.5).Figure 1: Ubbelohde capillary viscometer Figure 2: Viscometer with holderfor suspension in thermostatTable 1Capillary Measuring range,Viscometer Internal Internalsize no. in mPaconstant, K, diameter d1, diameter d2,in mPa in mm in mmIc 1,5 to 9 0,03 0

24、,63 5Ia 2,5 to 15 0,05 0,70 5II 5 to 30 0,1 0,84 5Iic 15 to 90 0,3 1,03 5Iia 25 to 150 0,5 1,25 5III 50 to 300 1 1,50 5IIIc 150 to 900 3 195 5IIIa 250 to 1 500 5 2,22 5IV 500 to 3 000 10 2,65 5IVc 1 500 to 9 000 30 3,47 8IVa 2 500 to 15 000 50 3,94 8V Above 5 000 100 4,70 8NOTE: All values are guide

25、line values.Page 4DIN 53177 : 2002-117.2 Equipment for producing a constant hydrostatic pressure of 58,8 hPaIn the assembly shown in figure 3, which has proved satisfactory in practice, constant hydrostatic pressure isproduced by injecting air via a three-way stopcock (1) set so that the air emerges

26、 at the funnel-shaped bottomend of the tube (2). Because the change in volume in the viscometer is negligible compared with the total volumeof air, the pressure will be sufficiently constant during measurement.Figure 3: Assembly to produce constant hydrostatic pressure7.3 Thermometer, having 0,1 C s

27、cale intervals (spaced at 0,6 mm) so that temperatures can be measuredto an accuracy of 0,05 C. In arbitration cases, only calibrated thermometers shall be used.7.4 Calibrated stopwatch, having time intervals of not more than 0,1 s. It shall be compared from time totime with a precision clock (accur

28、ate to t15 s per 24 h) and the spring shall not be too weakly tightened.7.5 Thermostat, with constant-temperature bath, capable of being controlled to within 0,05 C for tempera-tures between 15 C and 30 C and to within 0,1 C outside that range. The bath shall be protected from directsunlight or dire

29、ct artificial light, since this may falsify the temperature reading. The thermometer and bath shalltherefore be illuminated by low-radiation fluorescent tubes.8 Preparation for measurement8.1 Selection of viscometerThe viscometer shall be selected so that the time taken for the test liquid to flow f

30、rom measuring mark M1 tomark M2 is at least 50 s since otherwise the precision limits specified in clause 12 may be exceeded. The upperlimit of flow time will depend on the measuring ranges specified in table 1.8.2 Cleaning the viscometerBefore being used for the first time and from time to time the

31、reafter, the viscometer shall be cleaned with amixture of equal parts of concentrated sulfuric acid and saturated aqueous potassium dichromate solution (i.e.chromic acid) and then rinsed with distilled water and ethanol.NOTE: Given the known toxicity of chromium(VI) compounds, suitable cleaning conc

32、entrates have recentlybeen introduced.After use, the viscometer shall be emptied and cleaned with a suitable solvent (e.g. benzine, toluene, ethanol,acetone), acetone being used for the final rinse. The residual solvent shall be removed by sucking or blowinga dry, dust-free air stream through the vi

33、scometer.Page 5DIN 53177 : 2002-118.3 Determination of viscometer constantTo determine the viscometer constant, the flow time of standard oils whose dynamic viscosity is known to anaccuracy of 0,2 % shall be measured as specified in clause 8. The viscometer constant, K, in mPa, shall becalculated us

34、ing the following equation:K = th(1)whereh is the dynamic viscosity of the oil, in mPa. s;t is the flow time of the oil, in s.For viscosities up to 104mPa. s, pure mineral oils whose viscosity has been determined as specified (e.g. inaccordance with DIN 51562-1 to DIN 51562-3) may be used as standar

35、d oils2).NOTE: Since the Hagenbach correction is not applied in this standard, flow times of 50 s shall not be exceededunder any circumstances when determining the viscometer constant; for viscometers of size nos. Ic and Ia,standard oils having flow times of over 100 s shall, if possible, be used.9

36、ProcedureImmerse the viscometer in the temperature-controlled test liquid, with the straight end down, then applyvacuum to the bent end so as to suck in enough liquid to the bend adjacent to the capillary. After removing thevacuum and rotating the viscometer, attach a hose to the straight end and co

37、nnect it to a three-way stopcock(see figure 3). Close the stopcock when the liquid meniscus is about 1 cm to 2 cm below mark M1.Suspend the filled viscometer in the thermostat so that the level of the bath liquid is above mark M2 and themeasuring capillary is vertical.After waiting at least ten minu

38、tes (for measuring temperatures between 15 C and 30 C) or at least 20 minutes(for temperatures below 15 C and above 30 C), start the measurement. If the assembly shown in figure 3 isused to produce a constant hydrostatic pressure, inject air through the stopcock and adjust the hydrostaticpressure to

39、 58,8 hPa (equivalent to a 600 mm water column). Then connect the viscometer by rotating thestopcock and measure, to an accuracy of 0,1 s, the time required by the test liquid to rise from mark M1 tomark M2. This measurement may also be made using a light barrier or some other electronic device.Remo

40、ve the viscometer from the bath, empty it using vacuum and then clean and dry it as specified in sub-clause 8.2.10 EvaluationCalculate the dynamic viscosity, h, in mPa. s, using the following equation:h = K twhereK is the viscometer constant, in mPa;t is the flow time, in s.11 Precision11.1 Repeatab

41、ility limit(same operator, same equipment)The absolute difference between two successive results expressed as the mean of two results and obtainedunder repeatability conditions will not exceed the repeatability limit r, with a confidence level of 95 %. Accord-ing to this standard, r is 1 % for visco

42、sities of up to 5 000 mPa. s and 3 % for viscosities above that value.11.2 Reproducibility limit(different operators, different equipment)The absolute difference between two individual results expressed as the mean of two results and obtainedunder reproducibility conditions will not exceed the repro

43、ducibility limit R, with a confidence level of 95 %.According to this standard, R is 2 % for viscosities of up to 5000 mPa. s and 6 % for viscosities above thatvalue.2) Standard oils are obtainable from the Physikalisch-Technische Bundesanstalt (PTB), Bundesallee 100,38023 Braunschweig, Germany.Page

44、 6DIN 53177 : 2002-1112 Test reportThe test report shall refer to this standard and include the following details as a minimum:a) all the details required to identify the product tested (manufacturer, product designation, batch number,etc.);b) the temperature of the liquid under test, in C, to an accuracy of 0,5 C;c) the dynamic viscosity, in mPa. s, as a mean (with single values given in arbitration cases);d) any deviation from the test method specified;e) date of testing.