BS-EN-12595-2000 BS-2000-319-2000.pdf

| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 12595:2000 BS 2000-319:2000 The European Standard EN 12595:1999 has the status of a British Standard ICS 75.140; 91.100.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Methods of test for petroleum and its products Ð BS 2000-319: Bitumen and bituminous binders Ð Determination of kinematic viscosity (Identical with IP 319-2000) Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 July 2000 Institute of Petroleum and BSI 07-2000 ISBN 0 580 36078 4 BS EN 12595:2000 Amendments issued since publication Amd. No.DateComments National foreword This British Standard is the official English language version of EN 12595:1999. The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology, which has the responsibility to: Ð aid enquirers to understand the text; Ð present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; Ð monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. The Institute of Petroleum publishes and sells all parts of BS 2000, and all BS EN petroleum test methods that would be part of BS 2000, both in its annual publication ªStandard methods for analysis and testing of petroleum and related products and British Standard 2000 Partsº and individually. Further information is available from: The Institute of Petroleum, 61 New Cavendish Street, London W1M 8AR. Tel: 020 7467 7100. Fax: 020 7255 1472. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled ªInternational Standards Correspondence Indexº, or by using the ªFindº facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 15 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI (8523($1?67$1$5 1250(?(8523e(11( (8523b,6 for practical use, a submultiple (mm2/s) is more convenient. 3.2 density mass of a liquid divided by its volume NOTE: When reporting density, the unit of density used, together with the temperature, is stated explicitly, for example kilogram per cubic metre. 3.3 dynamic viscosity ratio between the applied shear stress and the velocity gradient NOTE 1: Dynamic viscosity is a measure of the resistance to flow of a liquid under gravity, and is commonly called the viscosity of the liquid. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 12595:1999 ?,QVWLWXWH?RI?3HWUROHXP?DQG?%6,? NOTE 2: The SI unit of dynamic viscosity is Pa·s. 3.4 newtonian liquid liquid having a viscosity that is independent of the rate of shear NOTE: The constant ratio of the shear stress to the velocity gradient is the viscosity of the liquid. If this ratio is not constant, the liquid is non-newtonian. 4 Principle The time for a fixed volume of the liquid to flow through the capillary of a calibrated glass capillary viscometer under an accurately reproducible head and at a closely controlled temperature is determined. The kinematic viscosity is calculated by multiplying the efflux time in seconds by the viscometer calibration factor. 5 Apparatus Usual laboratory apparatus and glassware, together with the following. 5.1 Viscometer, Cannon-Fenske, the Zeitfuchs Cross-Arm and BS/IP/RF viscometers, capillary-type, made of borosilicate glass, suitable for this method are described in Figures A.1, A.2 and A.3, and Tables A.1, A.2 and A.3. Other viscometers are allowed if test results obtained are comparable. Calibrated viscometers are available from commercial suppliers. Details regarding the calibration of viscometers are given in annex C. 5.2 Thermometers, calibrated liquid-in-glass, of an accuracy of 0,2 °C can be used or another thermometric device of equal accuracy as described in annex B. The specified thermometers shall be standardized at total immersion that is immersion to the top of the mercury column with the remainder of the stem and the expansion chamber at the top of the thermometer exposed to room temperature. NOTE 1: The practice of completely submerging the thermometer is not recommended. When thermometers are completely submerged, corrections for each individual thermometer based on calibration under conditions of complete submergence are determined and applied. If the thermometer is completely submerged in the bath during use, the pressure of the gas in the expansion chamber will be higher or lower than during standardization, and can cause a high or low reading on the thermometer. It is essential that liquid-in-glass thermometers be recalibrated periodically and that official corrections be adjusted as necessary to conform to any changes in temperature readings. The thermometer shall be read, estimating the reading to 0,1°C. NOTE 2: Thermometers should be checked at regular time intervals. NOTE 3: A commonly used procedure given in Method ASTM E 77 applies correction which is based on changes in the ice point calibration. Other temperature measuring devices may be used instead of mercury stem thermometers. However, the mercury stem thermometer is the reference device. Therefore any alternative device employed shall be calibrated so as to provide the same readings as would be provided by the mercury stem thermometer, recognizing and allowing for the fact of changed thermal response times compared with the mercury thermometer. NOTE 4: When measuring and controlling nominally constant temperatures as in this test method, alternative devices can indicate greater cyclic variations than mercury thermometers, to an extent depending on the cycle time of heating and the power of the controlled heat input. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 5 EN 12595:1999 ?,QVWLWXWH?RI?3HWUROHXP?DQG?%6,? 5.3 Bath, suitable for immersion of the viscometer so that the liquid reservoir or the top of the capillary, whichever is uppermost, is at least 20 mm below the upper bath level, and with provisions for visibility of the viscometer and the thermometer. Firm supports for the viscometer shall be provided, or the viscometer shall be an integral part of the bath. The efficiency of the stirring and the balance between heat losses and heat input shall be such that the temperature of the bath medium does not vary by more than 0,3 °C (measurement at 60 °C) or 0,5 °C (measurement at 135 °C) over the length of the viscometer, or from viscometer to viscometer in the various bath positions. Water, conforming to the grade 3 of EN ISO 3696, is a suitable bath liquid for determinations at 60 °C. USP white oil or any paraffinic or silicone oil with a flash point above 215 °C has been found suitable for determination at 135 °C. The flash point is determined in accordance with EN 22592. 5.4 Timer, stop watch (spring or battery driven) graduated in divisions of 0,1 s or less and accurate to 0,5 s over 1 000 s when tested over intervals of not less than 15 min. 5.5 Electrical timing devices, for use only on electrical circuits the frequencies of which are accurate to 0,5 s over 1 000 s or better. NOTE: Alternating currents, the frequencies of which are intermittently and not continuously controlled, as provided by some public power systems, can cause large errors, particularly over short timing intervals, when used to actuate electrical timing devices. 5.6 Automatic or semi-automatic equipment, are allowed providing that they meet the specifications for temperature regulation and time accuracy described in this clause and have been shown to achieve the same precision as given in clause 10 and are fully calibrated. 6 Preparation of test samples The laboratory sample shall be taken in accordance with EN 58. Prepare the sample in accordance with EN 12594. Bring the viscometer and the sample to within ±30 °C of the test temperature (in order to avoid correction of constants of the viscometer). Stir the sample thoroughly without entrapment of air. If the temperature has dropped to 30 °C or more below the test temperature, reheat the sample. Immediately charge the viscometer, or, if the test is to be made at a later time, pour approximately 20 ml into one or more clean, dry containers having a capacity of approximately 30 ml and immediately seal with an airtight closure. 7 Procedure 7.1 Test conditions Maintain the bath (5.3) at the test temperature to within ±0,3 °C (measurements at 60 °C) or ±0,5 °C (measurements at 135 °C). Apply the necessary corrections, if any, to all thermometer readings. Select a clean, dry viscometer giving an efflux time greater than 60 s and preheat it to the test temperature. Charge the viscometer in the manner dictated by the design of the instrument, as prescribed in the following. To charge the Cannon-Fenske opaque viscometer, invert the viscometer and apply vacuum to the tube L, immersing tube N in the liquid sample. Draw liquid through tube N, filling bulb D to fill mark G. Wipe excess sample off tube N and invert the viscometer to its normal position. Mount the viscometer in the constant temperature bath keeping tube L vertical. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 6 EN 12595:1999 ?,QVWLWXWH?RI?3HWUROHXP?DQG?%6,? Apply a stopper to the top of the apertures of tube L when bulb A is nearly 4/5 filled. Mount the BS/IP/RF viscometer in the constant temperature bath keeping tube L vertical. Pour sample through tube N to a point just above filling mark G; allow the sample to flow freely through capillary R, taking care that the liquid column remains unbroken, until the lower meniscus is about 5 mm below the filling mark H and then arrest its flow by closing the timing tube with a cork or rubber stopper in tube L. Add more liquid if necessary to bring the upper meniscus slightly above mark G. After allowing the sample to attain bath temperature and any air bubbles to rise to the surface, gently loosen the stopper allowing the sample to flow to the lower filling mark H and again arrest flow. Remove the excess sample above filling mark G by inserting the special pipet until its cork rests on top of tube N; apply gently suction until air is drawn through. The upper meniscus shall coincide with mark G. Mount the Zeitfuchs Cross-Arm viscometer in the constant temperature bath, keeping tube N vertical. Introduce sample through tube N, taking care not to wet the sides of tube N, into the cross-arm D until the leading edge stands within 0,5 mm of fill mark G on the siphon tube. 7.2 Determination and measurement Allow the viscometer to remain in the constant temperature bath for sufficient time to ensure that the sample reaches temperature equilibrium. Test shall be performed within 4 h. NOTE 1: Temperature equilibrium is not normally achieved for at least 30 min. Remove the stopper in tube L and allow the sample to flow by gravity until the lower meniscus is opposite the lower timing mark E. Measure to the nearest 0,1 s the time required for the leading edge of the meniscus to pass from timing mark E to timing mark F and from F to I (Cannon-Fenske). If this efflux time is less than 60 s, select a viscometer of smaller capillary diameter and repeat the operation. Upon completion of the test, clean the viscometer thoroughly by several rinsings with an appropriate solvent completely miscible with the sample, followed by a completely volatile solvent. Dry the tube by passing a slow stream of filtered dry air through the capillary for 2 min, or until the last trace of solvent is removed. Periodically clean the instrument with a suitable non-caustic cleaner to remove organic deposits, rinse thoroughly with water conforming to grade 3 of EN ISO 3696 and residue-free acetone, and dry with filtered dry air. NOTE 2: Use of alkaline glass cleaning solutions can result in a change of viscometer calibration, and is not recommended. 8 Calculation Calculate the kinematic viscosity, n, in millimetres squared per second, using results from different timing marks, using the following equation: n = C ? t where: Cis the calibration constant of the viscometer, in millimetres squared per square second; tis the efflux time, in seconds. Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 09:56:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 7 EN 12595:1999 ?,QVWLWXWH?RI?3HWUROHXP?DQG?%6,? 9 Expression of results Express the kinematic viscosity as the mean value, to three significant figures below 1 000 mm2/s or as the whole number above this value, together with the test temperature. 10 Precision 10.1 Repeatability The difference between two successive test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the value given in Table 1 in only one case in twenty. 10.2 Reproducibility The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method, exceed the value given in Table 1 in only one case in twenty. Table 1 - Precision values Repeatability r % of mean Reproducibility R % of mean at 135 °C 600 mm2/s ? 600 mm2/s at 60 °C soft bitumen soft bitumen after hardening (TFOT) ratio of kinematic viscosity at 60 °C (KV - ratio 1,5) 4 4 7 9 6 6 9 9 20 16 NOTE: These precision data are not automatically applicable to modified bitumen and for modified bitumen they should only be used for guidance, until criteria data are available. 11 Test report The te