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    Iso 2555-1989

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    Phạm Thu Huyền

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    © All Rights Reserved
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    INTERNATIONAL ISO STANDARD 2555 ‘Second edition 1989-02-01 Corrected and reprinted 1900.02.01 Plastics — Resins in the liquid state or as emulsions or dispersions — Determination of apparent viscosity by the Brookfield Test method Plastiques — Résines & état iquide ou en émmulsions ou dispersions — ‘Détermination de a viscosité apparante salon le Procédé Brookfield Reference number 180 2566 : 1989 (E) ISO 2565 : 1989 (E) Foreword 180 (the Intemational Organization for Standardization) is @ worldwide federation of national standards bodies (ISO member bodies). The work of preparing International ‘Standards is normally carried out through ISO technicel committees. Each member body interested in a subjact for which @ technical committee has been established has the right to be represented on that committee. International organizations, govern- ‘mental and non-governmental, in liaison with ISO, also take part in the work. ISO ‘collaborates closely with the International Electrotechnical Commission (IEC) on all ‘matters of electrotechnical standardization. Draft International Standards sdopted by the technicel committees are circulated to ‘the member bodies for approval before their acceptance as international Standards by the ISO Council. They are approved in accordance with ISO procedures requiring at least 75 % approval by the mamber bodies voting. International Standerd ISO 2565 was prepared by Technical Committee ISO/TC 61, Plastics. ‘This socond edition cancels and replaces the first edition (ISO 2556 : 1974), of which it constitutes a technical revision, ‘Annoxes A and B form an integral part of this International Standard. © International Organization for Standardization, 1989 © Printed in Switzriand INTERNATIONAL STANDARD 180 2555 ; 1989 (E) Plastics — Resins in the liquid state or as emulsions or dispersions — Determination of apparent viscosity by the Brookfield Test method") 1 Scope ‘This Intemational Standard specifies a method of determining ‘an apparant 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, ‘The application of this method to specific products is detailed in annex A, “The viscometer, types A, B and C, permit viscosity measure iments from 0,02 Pas (20 cP) to 6) 000 Pa (60 x 108 cP). 2 Principle A spindle, of cylindrical or related form (dsc, is driven at @ ‘constant rotational 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 the movement of noodle on a ci ‘The apparent viscosity by the Brookfield Test method is obtained bby mulipiyng ths dal reeding by a coefficient which depends on the rotational frequency and characteristics of the spindle. ‘The products to which this International Standard is applicable fare generally non-Newtonian and the measured viscosity depends on the velocity gradient to which the products are subjected duting the measurement. ‘With these types of viscometer, the velocity gradiant is not the same for every point of the spindle. Thus, for anon-Newtonian uid, the result is not strictly the true “viscosity at 3 known volocity 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 dotaiied working principle ofthis apparatus, its description and the characteristics of the three types are given in annex B. Each viscometer consiats of: — the viscometer body; — seven interchangeable spindles numbered from 1 to 7 (oumber 1 boing the largest); theso spindles carry a mark that indicates the immersion level in the liquid; they are the ‘seme for the three types of viscometer; do not use spindles which chow signe of eorracion or eceontricity; — 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 ofthe Brookfield apparatus, te relationship bo- ‘ween the models and avaliable frequencies and viscometer types A, B ‘and Care given in table 1. Othor rotational frequencies within the same limits may be chosen. Table 1 — Rotational frequencies available for the three types of viscomet acomtrT taodei | otaonl tequencte,min-* we PE) a [ven 0m 1a [avr [ow 7 ap 6 10 a “o 3 TRAE 1268 wat [05125 6 10 60 10) c fue fee net [os 1 28 6 0 2 #0 100 ‘The shapes and sizes of the spindles are such that the viscosities corresponding to @ maximum torque indication on the meter, for the various rotational frequencles, are thoso siven in table 2. ‘The adjustment and calibration of those viscomoters are usually carried out by the manufacturer of the apparatus. 1) The Brooklild Taet method may be cared aut using eet equipment suppiad by = numberof manufacturer 1SO 2565 : 1989 (E) Table 2 — Maximum value of viscosity (Pa-s) as a function of viscometer type, rotational frequency and spindle Vacomatr] Rotations ‘Spindle number GS min 1 2 3 4 5 6 7 100 or | 04 7 2 4 0) 4 80 02 | 08 2 4 8 | » os | 2 5] tw] 2 50 | 200 0 1 4 w | 2] 4 | 10} 0 A 5 2 8 nm] «| #9 | 20] 2 4 28 | 10 2 | so | 19 | 250 | 10 25 a | 4 | 9 | 1 | 40} 160 2 os | 2 so | 100 | 20} 800 | 200 1 w | # wo | 200 | 400 | 1000 | 4000 08 » | # 200 | 400 | eo | 2000 | 8.00 100 02 | 0B 2 4 8 2 80 0 o4 | 16 4 s| 16 40 | 160 2» 1 4 wo} 2 | «| 10) 0 0 2 8 o| {| » | 2/ a 8 5 4 8 40} 9 | 10 | 400 | 1600 25 8 | 2 so | 10 | sa | a0 | 320 2 w | 4 10 | 200 | 40 | 1000 | 4000 1 » | » 200 | 400 | 00 | 2000 | 8000 os | 16 400 | 00 | 1600 | 4000 | 16000 700 os | 32 | wl 2 20 | 320 0 ul ea] wl] | «| wo) oo 2 a | oe 4 | | 160 | 40} 100 10 a | 2 w | 10 | x0 | wo} 320 e 5 w | 6 10 | a2 | Go | 1600 | 6400 25 2 | we 30 | e40 | 1280 .| 3200 | 1200 2 0 | 160 400 | a0 | 1600 | 4000 | 16000 1 a | 20 00 | 1600 | 3200 | ac | 22000 08 too | 6% | 1600 | 20 | 6400 | 16000 | e+000 1) 1 Pas = 1090P It is recommended that the adjustment and caltration be checked from time to time by means of Newtonian liquids of known visoosity either by the user's laboratories or by official standardizing laboratories. 3.2 Thermostatic liquid bath, to maintain the product boing tested at tho test temperature with an accuracy of £0,2°C. Recommended test temperatures, in degroos Celsius, ara: 23, 25, 40, 65, 70, 85 and 100. NOTE ~ Ifthe test has to bo caried at higher temperatures, it sivieab to sine An extension shoft batwnon the spindle and the ‘epperats. 3.3 Additional apparatus 3.3.1 Support, which holds the viscometer and moves it in a vertical plane. 3.3.2 Beaker, 90 mm to 82 mm in diameter and 118 mm to 160 mm in height. 3.3.3. Thermometer, graduated in 0,1 °C, to measure the temperature of the product being tested, 4 Choice of rotational frequency and spindle Choose the rotational frequoncy-spindle combination taking into account the value of the viseosity 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 than 20 % or more than 95 % of full-scale deflection. However, for the best accuracy itis advisable to oop to the range 45 % to 95 % of full scale. 2 compatioon of viecesities betwoon non-Newtonian pro- ducts is desired, it is necessary to use the same rotational froquency-spindle combination for all the measurements, oven 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=" be used. ‘The rotational frequency-spindle combination to be used shall bbe specified in the document thet 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 96 % of full scale 5 Procedure Mount the viscometer, with its guard stirup, when applicable (ee sub-clause B.3.3 in annox 8) on its suppor. Fill the beaker (3.3.2) with the product to be tested, taking care not to introduce air bubbles, then place itn the bath (3.2) for a suffi- cient time to reach 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 boaker still in the bath, hold the spindle at an angle of approximately 45° to the surface of the product and immerse it In the product. Orientate 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 beakor and that the spindle is immersed to the underside of the mark on its shaft. Immerse the thermometer (3.3.3) in tho product Weit 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 manufacturer's roeommendatione. Allow the instrument to run and read the torque meter to the nearest 0,25 % of maximum value indication, in accordance with the manufacturer's recommendations, when a stable value hhae been reached on the metor. Lock the naedle and stop tho ‘motor to take the reading. noTes 1 if tho wading ofthe torque mater changes slowly this may indica that the product is thixotropic or sheopectic. The cocument that prescribes tho measurement (aoe annex A, clause A.1) should state Whether the reading of the torave meter should be taker after 2 Cefined ime, ors soon as i has become constant sso possible to plot the curve of viscosity asa function of period of rotation, 2_ Different liquids may have different rheology. For quid with 2 thixotropie or teopectic behaviour, the period of rotation should be fixed, 8.9. 1 min (use only 1 parod sinco the roading of the torque mater may depend co ti). Restart the motor and make another measurement, Continue taking measurements until two consecutive values ‘are obtained that do not differ by more than 3 % from each ‘other (unless otherwise specified in the documents mentioned in annex A, clause A.1). Tako tho average of these two values. After each determination, 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 Axkx! 1000 1SO 2555 : 1989 (E) where Ais a coefficient depending on the type of apparatus Whose value is 1 for type A, 2 for type B and 8 for type C; kis @ coefficient depending on the rotational frequency- spindle combination used; in the case of apparatus as specified in annex B, clause B.3, the valuos of k are as shown in table 3; 1 ig the mean of the two values read on the scale, Table 3 — Coefficient k (scale 0 to 100) for each rotational frequency-spindle combination) Rotational Cosfficiont & for spindle numb frequency] y | 2; a; a; eye) 7 rmin~1 | torgest |smateso} 100 1 | 4{ wl 2 «| 100/ ao 50 2 | 8| 2| 4/| | 20) 0 2 8 | 20] | 100} 200] s00| 2000 10 10 | 4 | 100] 200| 400| 1000] 4.000 5 20 | #0 | 200| 400] 800} 2000) 8000 4 25 | 100 | 250| 500 1 000 | 2 500) 10000 25 | 4 | 160 | 400/800] 1 600] 4 000] 18.000, 2 50 | 200 | s00| 1 000 | 2 000 | & 000| 20 000 1 | 100 | 400 | + 000 | 2.000 | 4 a00 |10 000) 40 o00 0.8 | 200 | 800 |2000 | 4 000 | & 000 [20 000| 80 000, 1) Ie may be necessary to calbrate each spindle with known viscosity and to adopt slightly diforant values of K (see cause 8.4 in annex 8) Express the results to three significant figures, indicating the type of viscometer (A, B oF C), the number of the spindle and the rotational frequency, as in the following example: Brookfield viscosity (A/3/20) = 4,25 Pars {1 Pass = 102 eP), NOTE ~ If the measurement has been made under the conditions “doscribod in the notes to louse & (thixotropie or rheonectie product fellow the spacial intnictions of the document mentioned in nex A, clause A.1. 7 Test report “The tast report shall include the following particulars 2}, a reference to this International Standard )_ the designation ofthe product being tested; ©} the test temperature; 4) the model of viecometer used; ©) the value of the apparent viscosity calculated in accord- ‘ance with the directions of clause 6. 1SO 2555 : 1989 (E) Annex A (normative) General application to resins in the liquid state, emulsions and dispersions A.1_ Field of application This annex shall be used for datormining the apparont viscosity Of resins in the liquid state, unless any indication to the contrary is given, It shall be used whenever a standard or a commercial contract ‘concerning the product recommends the use of ISO 2585 and its annex A. A2 Choice of test conditions A.2.1 Rotational frequency ‘Owing to the ganerally non-Newtonian behaviour of the prod- ucts covered by this ennex, the results obtained with different rotational frequencies cannot theoretically be compared. ‘The choice of the frequency deponds on the viscosity range to ‘bo maasured. It shall bo stated for each typo of product. It is necessary to establish a diagram showing the viscosity, tanga covered for the viscomater used at the spacifid fra- ‘quency (see figute A. 1 for an example of the diagram for visco- meters A, B and C at a frequency of 10 min") Hf the valuo of apparent viscosity to be measured is known ‘approximately, choose the spindle with the help of a diagram. (208 A.2.1), showing, for each type of viscometer, the range of viscosity covered by each spindle. For the comparison of results, itis better to keep the same spindle even if one must use it within a range wher its use is only “permitted”, than to work with different spindles. Practice shows that tho results are not aways the same between suc- cessive spindles. If the value of viscosity to be measured is not known, make measurements with successive spindles, beginning with number 7 until the requirements of figure A.1 are met. A.2.3 Particular conditions recommended for certain products Table A.1 summatizes the particular test conditions recom- mended for a number of products in the light of international practice. The spindle shall be chosen in accordance with the recommendations of clause 4 of this standard, taking into ac- ‘count the viscosity value. Table A.1 — Recommended test conditions Vireo. | Rote Product Visco | tional | Tomp- | Special moter | “free | erature | remarks awoncy mmin-t | 8c Phonic rina a | | 2 Polyester reine av | wo | 2 Epoxy resins ay | io | 2 Ahosives A» | 10020] 23 ‘Aquoous deporsions | A” | 5 | 2 PVC pastes av | om | 22 | rood ater L min, 1) Tho us of types 8 or C is alowed whan the viscosity of tho products greater than th sco it measurable with type A. the rotational requency recommend. ISO 2555 : 1989 (E) A3 Procedure If nocassary, bubbles can be eliminated by applying @ vacuum (or by any other appropriate method. Follow carofully the inetructiona given in clause 5. Take particular care only to measure the viscosity of products _In the case of products which are volatile, or have volatile con- completely free of bubbles. stituents, its, of course, necessary to use closed vessels, Viscosity, Pes" 01 05 1 5 10 50 100 500 1000 5 000 Figure A.1 — Viscosity range (logarithmic scale) for every spindle of the A. B and C viscometers ‘at a rotational frequency of 10 min~! Pas = 1 oP 1SO 2565 : 1989 (E) Annex B (normative) Principle, description and characteristics of viscometers A, B and C B.1_ Operating principle ‘The viscometer comprises a synchronous motor rotating a ‘vortical shaft through a goar-box. This vertical shaft drives, through a spiral spring, a second lower shaft, forming an extension of the first. A’ removable ‘spindle is attached to this second shaft and is immersed in the liquid under test. These two shafts rotate at the same frequency but, when the ‘spindle is immersed there is an angular deviation between them \which i a function of the liquid resistance to the rotation of the ‘spindle, ie. the liquid viscosity. This deviation is measured by a horizontal need, fixed to the spindle shaft, moving on a horizontal dial fixed to the first (motor) shaft and consequently rotating with this shaft. When ‘tho spindle is turning in alr, the neodlo correaponds to tho “0” ‘graduation on the dial. Bocause of the difficulty of taking readings while the naedie ‘and dial are both rotating, a dial-needie locking system allows, the reading to be takon after the motor has stopped. B.2 Brief description pine Steocernter oy osteo it ans esecti erate eng cchronous motor, geat-box with its rotational frequency change button, spiral spring, dial and needle, and dial-needie locking systern. ‘The interchangeable spindles have the form of cylinders or discs of polished motal fixod on a shaft. They can be usad on. the thres types of viscometer. ‘The guard stirup consists of a metal plate with a “U” form to protect the spindles. B.3 Characteristics B.3.1. Viscometer body 8.3.1.1 Rotational frequencies of the spindles 4 of 8 rotational froquencies according to the type of apparatus; the rotational frequencies are given in table 1. 8.3.1.2. Dial graduation From 0 to 100 in half-

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