11. Procedure
11.1 Manual Apparatus
11.1.1 Fill the test cup with the sample so that the top of the meniscus of the test specimen is level with the filling mark, and position the test cup on the center of the heating plate. The temperature of the test cup and the sample shall not exceed 56°C (100°F) below the expected flash point. If too much test specimen has been added to the cup, remove the excess using a syringe or similar device for withdrawal of fluid. However, if there is test specimen on the outside of the test cup, empty, clean, and refill it. Destroy any air bubbles or foam on the surface of the test specimen with a sharp knife or other suitable device and maintain the required level of test specimen. If a foam persists during the final stages of the test, terminate the test and disregard any results.

11.1.2 Solid material shall not be added to the test cup. Solid or viscous samples shall be heated until they are fluid before being poured into the test cup; however, the temperature of the sample during heating shall not exceed 56°C (100°F) below the expected flash point.

11.1.3 Light the test flame and adjust it to a diameter of 3.2 to 4.8mm (1/8 to 3/16 in.) or to the size of the comparison bead, if one is mounted on the apparatus (see Annex A1). (Warning - Gas pressure supplied to the apparatus must not be allowed to exceed 3 kPa (12 in.) of water pressure.) (Warning - Exercise care when using a gas test flame. If it should be extinguished it will not ignite the vapors in the test cup, and the gas for the test flame that then enters the vapor space can influence the result.) (Warning - The operator shall exercise care and take appropriate safety precautions during the initial application of the test flame since test specimens containing low-flash material can give an abnormally strong flash when the test flame is first applied.) (Warning - The operator shall exercise care and take appropriate safety precautions during the performance of this test method. The temperatures attained during this test, up to 400°C (752°F), are considered hazardous.)

NOTE11 - Some preliminary test flame applications during the initial heating phase may be useful in detecting whether unexpected volatile material is present in the sample. A typical interval is at the beginning of the initial heating phase and then every 10°C up to the standard test flame application temperature. See 11.1.5.

11.1.4 Apply heat initially at such a rate that the temperature as indicated by the temperature measuring device increases 5 to 17°C (9 to 30°F)/min. When the test specimen temperature is approximately 56°C (100°F) below the expected flash point, decrease the heat so that the rate of temperature rise during the last 28°C (50°F) before the flash point is 5 to 6°C (9 to 11°F)/min.

NOTE 12 - With low flash point material or with highly viscous material, it is advised to use the 5 to 6°C/min heating rate from the start of the test to the end.

11.1.5 Apply the test flame when the temperature of th test specimen is approximately 28°C below the expected flash point and each time thereafter at a temperature reading that is a multiple of 2°C. Pass the test flame across the center of the test cup at right angles to the diameter, which passes through the temperature measuring device. With a smooth, continuous motion, apply the test flame either in a straight line or along the circumference of a circle having a radius of at least 150 more or less 1 mm (6.00 more or less 0.039 in.). The center of the test flame shall move in a horizontal plane not more than 2mm (5/64 in.) above the plane of the upper edge of the test cup and passing in one direction only. At the time of the next test flame application, pass the test flame in the opposite direction of the preceding application. The time consumed in passing the test flame across the test cup in each case shall be approximately 1 more or less 0.1s.

NOTE 13 - Some automated apparatus pass the test flame in one single direction. Apparatus that operate in this manner will typically shut off the test flame gas after each application, return to the starting position without creating a draft near and over the test cup, and the test flame will be relighted in such a manner that no fuel gas enters the cup vapor space before the next test application.

NOTE 14 - When determining the flash point of asphalt, it is recommended to carefully move fully to one side, such as with a spatula, any surface film formed before each application of the ignition source. Available data indicate that higher flash point is observed for asphalt samples when surface film formed is not moved aside, compared to the flash point observed when the surface film is moved aside prior to the application of the ignition source.

NOTE 15 - An alternative to the moving aside of the formed surface film can be found in Appendix X1.

11.1.6 During the last 28°C (50°F) rise in temperature prior to the expected flash point, care shall be taken to avoid disturbing the vapors in the test cup with rapid movements or drafts near the test cup.

11.1.7 When a foam persists on top of the test specimen during the last 28°C (50°F) rise in temperature prior to the expected flash point, terminate the test and disregard any results.

11.1.8 Meticulous attention to all details relating to the test flame, size of the test flame, rate of temperature increase, and rate of passing the test flame over the test specimen is required for proper results.

11.1.9 When testing a sample whose expected flash point temperature is not known, bring the test specimen in the test cup to a temperature no greater than 50°C (122°F), or if the sample required heating to be transferred into the test cup, bring the test specimen in the test cup to that temperature. Apply the test flame, in the manner described in 11.1.5, beginning at least 5°C (9°F) above the starting temperature. Continue heating the test specimen at 5 to 6°C (9 to 11°F)/min and testing the test specimen every 2°C (5°F) as described in 11.1.5 until the flash point is obtained.

NOTE 16 - Flash point results determined in an unknown expected flash point mode should be considered approximate. This value can be used as the expected flash point when a fresh specimen is tested in the standard mode of operation.

11.1.10 Record, as the observed flash point, the reading on the temperature measuring device at the time the test flame causes a distinct flash in the interior of the test cup.

11.1.10.1 The sample is deemed to have flashed when a large flame appears and instantaneously propagates itself over the entire surface of the test specimen.

11.1.11 The application of the test flame can cause a blue halo or an enlarged flame prior to the actual flash point. This is not a flash point and shall be ignored.

11.1.12 When a flash point or fire point is detected during any preliminary test flame application, or on the first application of the test flame, see 11.1.5, the test shall be discontinued, the result discarded, and the test repeated with a fresh test specimen. The first application of the test flame with the fresh test specimen shall be at least 28°C (50°F) below the temperature found when the flash point was detected under the conditions in 11.1.12.

11.1.13 When the apparatus has cooled down to a safe handling temperature, less than 60°C (140°F), remove the test cup and clean the test cup and the apparatus as recommended by the manufacturer.

NOTE 17 - Exercise care when cleaning the apparatus so as not to damage or dislocate the automated flash detection system, when used, or temperature measuring device. See the manufacturer's instructions for proper care and maintenance.

11.1.14 To determine the flre point, continue heating the test specimen after recording the flash point such that the test specimen temperature increases at a rate of 5 to 6°C (9 to 11°F)/min. Continue the application of the test flame at 2°C (5°F) intervals until the test specimen ignites and sustains burning for a minimum of 5s. Record the temperature of the test specimen when the test flame, which caused the test specimen to ignite was applied. Sustain burning as the observed fire point of the test specimen.

11.1.15 When the apparatus has cooled down to a safe handling temperature, less than 60°C (140°F), remove the test cup and clean the test cup and the apparatus as recommended by the manufacturer.

11.2 Automated Apparatus
11.2.1 The automated apparatus shall be capable of performing the procedure as described in 11.1, including control of the heating rate, application of the test flame, detection of the flash point, or fire point, or both, and recording the flash point or fire point, or both.

11.2.2 Fill the test cup with the sample so that the top of the meniscus of the test specimen is level with the filling mark, and position the test cup on the center of the heating plate. The temperature of the test cup and the sample shall not exceed 56°C (100°F) below the expected flash point. If too much test specimen has been added to the cup, remove the excess using a syringe or similar device for withdrawal of fluid; however, if there is test specimen on the outside of the test cup, empty, clean, and refill it. Destroy any air bubbles or foam on the surface of the test specimen with a sharp knife or other suitable device, and maintain the required level of test specimen. If a foam persists during the final stages of the test, terminate the test, and disregard any results.

11.2.3 Solid material shall not be added to the test cup. Solid or viscous samples shall be heated until they are fluid before being poured into the test cup; however, the temperature of the sample during heating shall not exceed 56°C (100°F) below the expected flash point.

11.2.4 Light the test flame, when necessary, and adjust it to a diameter of 3.2 to 4.8mm (1/8 to 3/16 in.) or to the size of the comparison bead, if one is mounted on the apparatus. (Warning - Gas pressure supplied to the apparatus must not be allowed to exceed 3 kPa (12 in.) of water pressure.) (Warning - Exercise care when using a gas test flame. If it should be extinguished it will not ignite the vapors in the test cup, and the gas for the test flame that then enters the vapor space can influence the result.) (Warning - The operator shall exercise care and take appropriate safety precautions during the initial application of the test flame since test specimens containing low-flash material can give an abnormally strong flash when the test flame is first applied.) (Warning - The operator shall exercise care and take appropriate safety precautions during the performance of this test method. The temperatures attained during this test, up to 400°C (752°F), are considered hazardous.)

NOTE18 - Some automated apparatus can perform preliminary test flame applications during the initial heating phase.

NOTE19 - Some automated apparatus can light the test flame automatically and the size of the flame is preset.

11.2.5 Start the automated apparatus according to the manufacturer's instructions. The apparatus shall follow the procedural details described in 11.1.4 through 11.1.15.