1、DEUTSCHE NORM Januarv 2000 Resins in the liquid state or as emulsions or dispersions Determination of apparent viscosity by the Brookfield Test method - EN IS0 2555 (IS0 2555 : 1989) English version of DIN EN IS0 2555 ICs 83.080.1 O Kunststoffe - Harze im flssigen Zustand, als Emulsionen oder Disper
2、sionen - Bestimmung der scheinbaren Viskositt nach dem Brookfield-Verfahren (IS0 2555 : 1989) European Standard EN IS0 2555 : 1999 has the status of a DIN Standard. A comma is used as the decimal marker. National foreword This standard has been published in accordance with a decision taken by CEN/TC
3、 249 to adopt, without alteration, International Standard IS0 2555 as a European Standard. The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Technical Committee Physikalische, rheologische und analytische Prfungen. EN comprise
4、s 9 pages. No pari of this standard may be reproduced without the prior permission of Ref. No. DIN EN IS0 2555 : 2000-0 Y Deutsches Institut frNonunge. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, s the exclusive right of sale for German Standards (DIN-Normen). English price group 08 Sales
5、No. 1108 06.00 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 2555 June 1999 ICs 83.080.1 O English version Plastics Determination of apparent viscosity by the Brookfield Test method (IS0 2555 : 1989) Resins in the liquid state or as emulsions or dispersions Plastiques - Rsines ltat liquid
6、e ou en mulsions ou dispersions - Dtermination de la viscosit apparente selon le Procd Brookfield (IS0 2555 : 1989) Kunststoffe - Harze im flssigen Zustand, als Emulsionen oder Dispersionen - Bestimmung der scheinbaren Viskositt nach dem Brookfield-Verfahren (IS0 2555 : 1989) This European Standard
7、was approved by CEN on 1999-05-06. CEN members are bound to comply with the CENKENELEC Internal Regulations 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 natio
8、nal stand- ards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist 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 no
9、tified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Swi
10、tzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels O 1999. CEN - All rights of exploitation in any form and by any means reserved worldwide for CEN nationa
11、l members. Ref. No. EN IS0 2555 : 1999 E Page 2 EN IS0 2555 : 1999 Foreword International Standard IS0 2555 : 1989 Plastics - Resins in the liquid state or as emulsions or dispersions - Determination of apparent viscosity by the Brookfield Test method, which was prepared by ISO/TC 61 Plastics of the
12、 International Organization for Standardization, has been adopted by Technical Committee CEN/TC 249 Plastics, the Secretariat of which is held by IBN, as a European Standard. This European Standard shall be given the status of a national standard, either by publication of an identical text or by end
13、orsement, and conflicting national standards withdrawn, by December 1999 at the latest. In accordance with the CENKENELEC Internal Regulations, the national standards organizations of the follow- ing countries are bound to implement this European Standard: Austria, Belgium, the Czech Republic, Denma
14、rk, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom. Endorsement notice The text of the International Standard IS0 2555 : 1989 was approved by CEN as a European Standard without any modificat
15、ion. Page 3 EN IS0 2555 : 1999 HBF HBT C 1 Scope This International Standard specifies a method of determining an apparent viscosity, by the Brookfield Test method, of resins in a liquid or similar state, using one of the types of rotational viscometer described in this Standard. 12 510 0.5 1 2,5 5
16、10 20 50 100 The application of this method to specific products is detailed in annex A. The viscometers, types A, B and C, permit viscosity measure- ments from 0.02 Pa.s (20 cP to 60 O00 Pa-s (60 x 106 cP). 2 Principle A spindle, of cylindrical or related form (disc), is driven at a constant rotati
17、onal frequency in the product being studied. The resistance exerted by the fluid on the spindle, which depends on the viscosity of the product, causes a torque which is indicated by a suitable meter. This measurement may be based on tightening of a spiral spring depending on the torque, indicated by
18、 the movement of a needle on a dial. The apparent viscosity by the Brookfield Test method is obtained by multiplying this dial reading by a coefficient which depends on the rotational frequency and characteristics of the spindle. The products to which this International Standard is applicable are ge
19、nerally non-Newtonian and the measured viscosity depends on the velocity gradient to which the products are subjected during the measurement. With these types of viscometer, the velocity gradient is not the same for every point of the spindle. Thus, for a non-Newtonian fluid, the result is not stric
20、tly the true “viscosity at a known velocity gradient“ and therefore is conventionally called the apparent viscosity. 3 Apparatus 3.1 Brookfield-type viscometer, type A, B or C, chosen according to the product to be tested and the desired precision. The detailed working principle of this apparatus, i
21、ts description and the characteristics of the three types are given in annex B. Each viscometer consists of: - the viscometer body; - seven interchangeable spindles numbered from 1 to 7 (number 1 being the largest); these spindles carry a mark that indicates the immersion level in the liquid; they a
22、re the same for the three types of viscometer; do not use spindles which show signs of corrosion or eccentricity; - a detachable guard stirrup (type A only). The rotational frequencies available on the different types of Brookfield Viscometer are given in table 1. NOTE - In the case of the Brookfiel
23、d apparatus, the relationship be- tween the models and available frequencies and viscometer types A, B and C are given in table 1. Other rotational frequencies within the same limits may be chosen. Table 1 - Rotational frequencies available for the three types of viscometer I I Model I Rotational fr
24、equencies, min Viscometer A B REI- 71 0.5 1 2.5 5 10 20 50 100 I HAT 10,s 1 2,5 5 10 20 50 1001 The shapes and sizes of the spindles are such that the viscosities corresponding to a maximum torque indication on the meter, for the various rotational frequencies, are those given in table 2. The adjust
25、ment and calibration of these viscometers are usually carried out by the manufacturer of the apparatus. 1) The Brookfield Test method may be carried out using test equipment supplied by a number of manufacturers Page 4 EN IS0 2555 : 1999 Table 2 - Maximum value of viscosity iPa.sl *I as a function o
26、f viscometer type, rotational frequency and spindle Viscometer type A 3 C Rotational frequency min 1 1 O0 50 20 10 5 4 25 2 1 0.5 100 50 20 10 5 2.5 2 1 0.5 100 50 20 10 5 25 2 1 0,s *) 1 Pa.s = lO3cP 1 o, 1 0.2 0,5 1 2 2,s 4 5 10 20 0.2 1 2 4 8 10 20 40 0,4 0.8 1.6 4 8 16 32 40 80 160 2 0.8 2 4 8 1
27、0 16 20 40 80 0,4 0.8 13 4 8 16 32 40 80 160 3.2 6.4 16 32 64 128 160 320 640 Spindle number 3 1 2 5 10 20 25 40 50 1 O0 200 2 4 10 20 40 80 1 O0 200 400 8 16 40 80 160 320 400 800 1 600 4 2 4 10 20 40 50 80 100 200 400 4 8 20 40 80 160 200 400 800 16 32 80 160 320 640 800 1 600 3 200 5 4 8 20 40 80
28、 100 160 200 400 800 8 16 40 80 1 60 320 400 800 1 600 32 64 160 320 640 1 280 1 600 3 200 6 400 6 10 20 50 1 O0 200 250 400 500 1 o00 2 O00 20 40 100 200 400 800 lo00 2000 4 O00 80 160 400 800 1600 3 200 4 O00 8 O00 16 000 7 40 80 200 400 800 1000 1600 2000 4000 8000 80 160 400 800 1 600 3 200 4 00
29、0 8 O00 16 000 320 640 1600 3 200 6 400 12 800 16 O00 32 O00 64 000 It is recommended that the adjustment and calibration be checked from time to time by means of Newtonian liquids of known viscosity, either by the users laboratories or by official standardizing laboratories. 3.2 Thermostatic liquid
30、 bath, to maintain the product being tested at the test temperature with an accuracy of I 0,2 oc. Recommended test temperatures, in degrees Celsius, are : 23, 25, 40, 55, 70, 85 and 100. NOTE - If the test has to be carried at higher temperatures, it IS advisable to use an extension shaft between th
31、e spindle and the apparatus. 3.3 Additional apparatus 3.3.1 vertical plane. Support, which holds the viscometer and moves it in a 3.3.2 160 mm in height. Beaker, 90 mm to 92 mm in diameter and 115 mm to 3.3.3 Thermometer, graduated in 0,l “C, to measure the temperature of the product being tested. 4
32、 Choice of rotational frequency and spindle Choose the rotational frequency-spindle Combination taking into account the value of the viscosity to be measured, the desired precision and the velocity gradient. It is necessary to make this choice in such a way that no measurement cor- responds to less
33、than 20 % or more than 95 % of full-scale deflection. However, for the best accuracy it is advisable to keep to the range 45 % to 95 % of full scale. If a comparison of viscosities between non-Newtonian pro- ducts is desired, it is necessary to use the same rotational frequency-spindle combination f
34、or all the measurements, even if the accuracy of one of the measurements is markedly decreased. The choice of rotational frequency automatically involves the choice of one or more types of viscometer. In this connection, it is recommended that, if possible, a rotational frequency of 10 min -1 be use
35、d. The rotational frequency-spindle combination to be used shall be specified in the document that prescribes the measurement (see annex A, clause A. 1). The choice may be made in terms of the stated or expected viscosity, using table 2 and noting that the most suitable range is between 45 % and 95
36、70 of full scale. 5 Procedure Mount the viscometer, with its guard stirrup, when applicable (see sub-clause 8.3.3 in annex B) on its support. Fill the beaker (3.3.2) with the product to be tested, taking care not to introduce air bubbles, then place it in the bath (3.2) for a suffi- cient time to re
37、ach the desired temperature. If the product con- tains volatile matter or is hygroscopic, take care to close the beaker tightly during this operation. With the beaker still in the bath, hold the spindle at an angle of approximately 45O to the surface of the product and immerse it in the product. Ori
38、entate the spindle vertically, and connect it to the shaft of the apparatus. Check that the spindle is vertical, using the bubble level, that the lower end of the spindle is more than 10 mm from the bottom of the beaker and that the spindle is immersed to the underside of the mark on its shaft. Imme
39、rse the thermometer (3.3.31 in the product. Wait until the temperature of the product is between the prescribed limits. Start the motor and run at the desired rota- tional frequency, taking into account the manufacturers recommendations. Page 5 EN IS0 2555 : 1999 where Allow the instrument to run an
40、d read the torque meter to the nearest 0.25 % of maximum value indication, in accordance with the manufacturers recommendations, when a stable value has been reached on the meter. Lock the needle and stop the motor to take the reading. NOTES 1 If the reading of the torque meter changes slowly, this
41、rnay indicate that the product is thixotropic or rheopectic. The document that prescribes the measurement (see annex A, clause A. 1) should state whether the reading of the torque meter should be taken after a defined time, or as soon as it has become constant. It IS also possible to plot the curve
42、of viscosity as a function of period of rotation. 2 Different liquids may have different rheology. For liquids with a thixotropic or rheopectic behaviour, the period of rotation should be fixed, e.g. 1 min (use only 1 period since the reading of the torque meter may depend on time). Restart the moto
43、r and make another measurement. Continue taking measurements until two consecutive values are obtained that do not differ by more than 3 YO from each other (unless otherwise specified in the documents mentioned in annex A, clause A.1). Take the average of these two values. After each determination,
44、detach the spindle from the apparatus and wash it thoroughly in a suitable solvent. 6 Expression of results Calculate the apparent viscosity, in pascal seconds, of the product tested, using the formula Axkxl A is a coefficient depending on the type of apparatus whose value is 1 for type A, 2 for typ
45、e B and 8 for type C; k is a coefficient depending on the rotational frequency- spindle combination used; in the case of apparatus as specified in annex B, clause 8.3, the values of k are as shown in table 3; I is the mean of the two values read on the scale. Table 3 - Coefficient k (scale O to 100)
46、 for each rotational frequency-spindle combination 1 10 10 20 4 25 2.5 40 2 50 100 0.5 200 Coefficient k for spindle number 2 - 4 8 20 40 80 1 O0 160 200 400 800 3 - 10 20 50 1 o0 200 250 400 500 1 O00 2 000 4 - 20 40 100 200 400 500 800 lo00 2o00 4 O00 1) it rnay be necessary to calibrate each spin
47、dle with liquids of known viscosity and to adopt slightly different values of k (see clause 6.4 in annex E). Express the results to three significant figures, indicating the type of viscometer (A, B or C), the number of the spindle and the rotational frequency, as in the following example : Brookfie
48、ld viscosity iA/3/20) = 4,25 Pa.s (1 Pa-s = lO3cPJ. NOTE - If the measurement has been made under the conditions described in the notes to clause 5 (thixotropic or rheopectic products), follow the special instructions of the document mentioned in annex A, clause A.l. 7 Test report The test report sh
49、all include the following particulars: a) b) c) the test temperature; a reference to this International Standard; the designation of the product being tested; di the model of viscometer used; lo00 e) ance with the directions of clause 6. the value of the apparent viscosity calculated in accord- Page 6 EN IS0 2555 : 1999 visco- meter type Product Annex A (normative) Rota- tional Temp- Special fre- erature remarks quency General application to resins in the liquid state, emulsions and dispersions A.l Field of application This annex shall be used for determi
