ASTM D7345 Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method)
12. Procedure
12.1 Material with an Initial Boiling Point of 100 °C and Below - Bring the temperature of the sample and container to a temperature at least 10 °C below the expected initial boiling point of the material before opening the sample container.
12.2 Material with a Boiling Point above 100 °C - Bring the sample and its container to ambient temperature. If the sample has partially or completely solidified during storage warm until fluid, then mix by gentle shaking.
NOTE 3 - Not respecting the requirements given in 12.1 can lead to improper IBP detection on samples containing volatile materials. If expected initial boiling point of the sample to be tested is unknown, it is advised to make a test at ambient conditions. If the distillation result shows that the requirements of 12.1 were not respected, discard the result and repeat the test strictly respecting the conditions.
12.3 Ensure that the distillation measuring head of automatic apparatus has been allowed to reach ambient temperature and that any residual condensate has been removed.
12.4 Check that the distillation flask is clean and dry.
12.5 Place at least 10 grains of clean and dry granular pumice stones into the distillation flask. Some apparatus supply a suitable boiling stone dispenser. When the sample is biodiesel (B100), do not use any pumice stones.
12.6 Measure 10 mL +/- 0.3 mL test portion using the sampling device (see Section 6). When the sample is biodiesel (B100), measure 5 mL +/- 0.3 mL test portion. Check for the presence of any bubbles and if present discard the test portion and refill with bubble free material. Transfer the bubble free test portion to the prepared distillation flask, taking care that none of the liquid flows into the vapor tube.
NOTE 4 - Use new disposable syringe or disposable dispenser tip for each new sampling to avoid any products cross contamination which can cause erroneous distillation results.
12.7 Fit the distillation measurement head into its position on the distillation flask securely in accordance with the manufacturer's instructions.
12.8 Place the distillation flask into the heating enclosure and insert the sidearm of the distillation flask into the sealing of the condenser tube, while also attaching the measurement head holder.
12.9 Position the heating source/flask support around the lower section of the distillation flask.
12.10 Close heating enclosure by positioning the protection shield to its position.
12.11 Check that a waste collection beaker is placed under the projecting lower end of the condenser tube. Ensure that the waste collection beaker remains open to atmospheric pressure.
NOTE 5 - Monitor that the liquid level in the waste beaker does not exceed two thirds of its total capacity and drain it on periodic intervals.
12.12 Without delay initiate the distillation process according to the apparatus manufacturer's instructions.
12.12.1 From this point up to and including the termination of the measurement, the apparatus automatically controls all operations. The instrument applies heating to the specimen and regulates automatically heating power during the distillation run using specimen liquid temperature data. The distillation conditions; distillation flask internal pressure, specimen liquid temperature, and specimen vapor temperature are automatically measured and recorded during the test by the control system. The distillation is automatically terminated when the flask internal pressure returns to its initial pressure level. The collected test data is automatically processed and reported on the display and printed out at the conclusion of the test run. The heating enclosure cooling fan is automatically activated.
12.13 Record the test data.
12.14 Allow the distillation flask to cool and remove it from the apparatus.
