GULF STANDARD U.A.E, STANDARD No. S01/1994 No. S01/1995 “PAINTS AND VARNISHES — METHODS OF TEST — DETERMINATION OF FLASH POINT — (CLOSED CUP METHOD)” United Arab EmiratesStandardization & Metrology Organization for G.C.C. (GSMO) P.O. Box - 85245 RIYADH - 11691 “PAINTS AND VARNISHES — METHODS OF TEST — DETERMINATION OF FLASH POINT — (CLOSED CUP METHOD)” Ics 87.040 This Standard is issued on the basis of the decision of the Board of Directors in accordance with the decision of the Supreme Council of the G.C.C. States in its Third Session, held in Bahrain on 1403-01-23 (corresponding to 1982-11-09). Date of Board of Directors’ Approval 13-06-1415 Corresponding to 16-11-1994 Date of Publication in the Official Gazette Corresponding to Date of Enforcement Corresponding to All rights reserved to this organizationGULF STANDARD GS 501/1994 “PAINTS AND VARNISHES — METHODS OF TEST — DETERMINATION OF FLASH POINT — (CLOSED CUP METHOD)” INTRODUCTION This Gulf standard describes the method of test and sampling for paints, varnishes and related products. It should be read in conjunction with the Gulf standard on “Paints and Varnishes - Methods of Test - Determination of Danger Classification by Flash Point - (Closed Cup Method)’. By this procedure, differences between test apparatus of various standard designs are minimized by ensuring that the test is carried out only when the product under test and the air/vapour mixture above it in the test vessel are approximately in temperature equilibrium, 1- SCOPE This standard specifies a method for determining the flash point of paints, varnishes and related products when tested by this method. This method is suitable for use with temperatures ranging between 5 and 65°C, although some of the apparatus cannot cover all this range on using the thermometer supplied with the apparatus. This method allows for necessary corrections of deviations in atmospheric pressure. 2- COMPLEMENTARY REFERENCES 2.1 Draft Gulf standard on ... “Paints and Varnishes - Sampling”. 2.2 Draft Gulf standard on of Samples for Testing” “Paints and Varnishes - Examination and Preparation 23° Draft Gulf standard on.../.... “Paints and Varnishes, Petroleum and Related Products - Flash/no Flash Point Test - (Closed Cup Equilibrium Method)”. 24 Draft Gulf standard on ..../.... “Petroleum Products - Liquid Hydrocarbons - Manual Sampling”. 2.5 Draft Gulf standard on .../..... “Petroleum Products - Liquid Hydrocarbons - Automatic pipeline Sampling”.GULF STANDARD GS 501/1994 2.6 Draft Gulf standard on .. “Paints, Varnishes, Petroleum and Related Products - Determination of Flash Point - (Rapid Equilibrium Method)". 3- DEFINITIONS Flash point (closed cup): Minimum temperature in C. measured at an air pressure of 101.3 KN/M2, at which air/vapour mixture may be ignited on bringing an external flame close to the solvent vapour (of the product under test) retained in a closed cup under test conditions. Note: Measurement of the flammability of the solvent vapour by extemal ignition indicates the degree of the product flammability hazards. 4- PRINCIPLE Ina suitable waterbath the test sample is heated in a closed cup to the required temperature level. The temperature of both the water bath and the test sample is slowly raised at such a rate that the difference in temperature between the liquid in the bath and the test sample never exceeds 2°C. A slow rate of heating is necessary because of the low thermal conductivity of paints, varnishes and related products, and also because heat transfer by convection is hindered by the high viscosity of most of these products. Thermal conductivity of the product under test may be assisted by the use of a stirring device, but stirring should be stopped on carrying out an ignition trial, During the heating-up period, ignition trials are carried out at intervals of not less than 1.5 min, This time interval is necessary to ensure that saturation of vapour in the air space above the test sample is re-established after each ignition trial. The above-mentioned heating up method ensures that temperature of the test sample is not raised by more than 0.5°C per one minute and half. 5- APPARATUS 5.1 Test cup ‘The test cup shall be of the closed type with an internal level indicator. Use Pensky- Martens apparatus for this purpose or any other similar equipment (see Gulf standard No. “Paints and Varnishes - Determination of Danger Classification by Flash Point - (Closed Cup Method)”. Note: If the test cup used is equipped with a stirrer, it may be operated during the heating- up period but should be stopped during the ignition trial. If stirrer originally fitted to the test cup is removed, the aperture in the cover should be securely plugged before starting the test. The test cup shall be fitted with a cover on an opening in aGULF STANDARD GS 501/1994 52 53 54 sliding section, capable of introducing the ignition device flame on opening the sliding section (diameter 3.5 + 0.5 mm). The nozzle of ignition device shall be + 1 mm above the under surface of cover. The ignition trial may be performed by opening the sliding section and inserting and removing the nozzle of the ignition device, and closing the sliding section again, in period of 2.5 4 0.5 s. An automatically driven device may be used for this purpose, Any suitable flammable gas can be used in the ignition device. Water bath Any suitable water bath capable of being adjusted to the required temperature (7.2.1.2) and of adequate heat capacity to meet the requirements of (7.2.3.5) can be used. A bath fitted with a stirrer and a self adjusted thermostat can be used. Thermometers The test cup shall be fitted with a thermometer of appropriate range, dimensions and accuracy that, when immersed in the test sample, measures its temperature. The water bath shall be fitted with a thermometer to measure water temperature. ‘Support For holding the test cup in the bath, a support shall be provided so that the cover and ‘upper edge of the cup be horizontal. The cup is immersed in direct contact with the water in the bath so as to have the level of the test sample in the cup same as that of the water in the bath. 6- SAMPLING AND CONDITIONING OF THE TEST SAMPLE 61 62 Take a representative test sample and condition it according to the methods specified in the Gulf standard mentioned in 2.2. Keep the sample in an airtight container. Because of the possibility of loss of volatile constituents, the test sample should be treated in the least possible time to ensure homogeneity. Directly after removal of the test sample, the sample container shall be tightly closed to ensure that loss of volatile components from the container is minimized, otherwise, a completely new sample will be necessary for carrying out other tests. 7- PROCEDURE al 72 721 Preliminary test Determine the approximate flash point of the sample by one or more preliminary tests. This test shall determine the starting temperature for the definitive test, which shall be about 5°C below the expected value. Definitive test Preparation of apparatusGULF STANDARD GS 501/1994 TQ T2A12 7213 722 7224 72.22 723 723.1 723.2 723.3 7234 723.5 Setup the apparatus in a draught-free position in a room controlled at 20°C. Adjust temperature of the water bath to 5°C below the approximate flash point as determined in 7.1. Carefully clean and dry the test cup, its cover and thermometer. Bring them to approximately the same temperature as that of the water bath in 7.2.1.2. ‘Test sample Take and prepare the test sample in accordance with item (6), ensuring at all times during this preparation ensuring at all times during this preparation that the temperature of the test sample is at least 10°C below the expected flash point temperature. Fill the test cup with the test sample until the internal level indicator just disappears under the liquid surface. Avoid both formation of bubbles and contact between the sample and the cup wall above the level indicator. If this significantly occurs, empty the cup, prepare it again as in 7.2.1.3, and fill it with a fresh test sample, Determination Immediately after filling the test cup, place the cover in position. Support the cup in the bath so that the cover is horizontal and the cup is immersed in direct contact with the liquid in the water bath until the test sample surface is at the same or below the level of the liquid in the bath, Ensure that the bath temperature is as defined in 7.2.1.2. Light the flame of the ignition device and adjust it to an approximately spherical shape of diameter 3.5 + 0.5 mm. ‘As soon as the test sample has attained the same temperature as that of the liquid in the water bath (i.e. the starting temperature of the definitive test), perform an ignition by opening the sliding section, inserting and removing the nozzle of the ignition device, and closing the sliding section again, over a period of 2.5 + 0.5. If ignition occurs and the resultant temperature is very high (see note to 7.2.3.5), carry out the procedure (7.2.3) again with a fresh test sample at a temperature lower by 5°C. If no ignition occurs (see note in this item), heat the bath at a rate such that the difference in temperature between the bath and the test sample never exceeds 2°C. If the test sample temperature increases by 0.5°C (or afier a period not less than 1.5 min.), repeat the ignition test. If no flash is observed repeat the procedure until a temperature degree is reached at which a flash occurs. Read temperature degree to the nearest 5°C for indicator cup thermometer, correct this reading for any known temperature corrections, and record the result as the temperature of flash point at the atmospheric pressure prevailing during the test. Also record the atmospheric pressure in kilonewton/m?, millibars or millimetres of mercury.GULF STANDARD GS 501/1994 Note: When the vapour mixture is near the flash point, application of the ignition flame may give tise to candescence, however, the product is only deemed to have flashed if a comparatively large blue flame appears and propagates itself over the surface of liquid. If a large blue flame appears as a flash, when the sliding section is opened and the ignition flame is introduced, then the flash point of the product is considerably below the test temperature, and determination should be repeated as from (7.1). 8- CALCULATION OF THE CORRECT FLASH POINT Calculate the correct flash point to standard atmospheric pressure of 101.3 kilonewton/m?2 (1013 millibars, 760 millimeter mercury), by adding the correction given in celsius algebrically to the observed temperature by one of the following equations 101.3 - Py 1013 - P, 760 - P3 - or « 30 Where: P} is the atmospheric pressure, expressed in KN/m2. P2_ is the atmospheric pressure, expressed in millibars. P3_ is the atmospheric pressure, expressed in millimeters of mercury. 9. PRECISION 9.1 9.2 Repeatability (one operator or equipment) : +2°C. Reproducibility (several operators or equipment) : + 3°C. Note: A preferable precision level is required for reference tests. The method mentioned in item (11) shall be followed.GULF STANDARD GS 501/1994 10- TEST REPORT The test report shall include the following information: 1) Arreference to this standard. 2) Type of the product tested. 3) Areference to the standard describing the test cup used, and details of any modifications introduced, 4) Correct flash point, calculated as in item 8. 5) Any deviation, by agreement or otherwise, from the test shall be defined. 6) The date of test. 1- REFERENCE TESTS Wal 1.2 4 1S Two or more of the reference individual measurements shall be carried out. If the difference between the results of two individual tests, according to item 8, does not exceed 1.0°C, report the mean value as the flash point, If the difference between the first two results exceeds 1.0°C, a third test shall be made. If the greatest difference between the three results does not exceed 1.5°C, report the mean value as the flash point. If the greatest difference between the first three results exceeds 1.5°C, two further tests shall be made. If only one of the five results differs by more than 1.5°C from the mean value, reject this result and report the mean value of the other four results as the flash point. If more than one of the five results differ by more than 1.5°C from the mean value, report this mean value as the flash point. Also report the individual values adding a note to the test report on the irregular flashing of the sample.