ASTM D1266 Test Method for Sulfur in Petroleum Products (Lamp Method)
10. Procedure for Blending and Combustion of Liquid Samples
10.1 Add 6 mL of sulfur-free diluent to each flask. Stopper the flasks with numbered corks and weigh to the nearest 0.005 g. By means of a pipet, introduce into the flask of each burner an approximate quantity of sample as indicated in Table 2; swirl to mix thoroughly, and reweigh.
NOTE 10 - Alternatively, make a quantitative 40 % blend of the sample in sulfur-free diluent and proceed as described in Section 9.
10.2 Insert the burner and burn as described in 9.2. Remove each lamp from its chimney as the flame nears extinction and extinguish the flame. Add 2 mL of diluent, allowing the diluent to rinse down the walls of the flask. Burn the additional diluent and repeat the addition of diluent and burning one more time so that a total of 10 mL of diluent has been burned.
NOTE 11 - In this case, it is desirable that a 10-mL diluent blank be run; the titration of the absorber solution from this blank, shall not exceed 0.1 mL of 0.05 M NaOH solution.
10.3 After all lamps have completed burning, turn off the CO2 and O2 supplies, close the connection to the vacuum regulator, draw air through the absorbers for 5 min, and finally close the vacuum control valve. Rinse the chimneys and spray traps three times, using about 10 mL of water each time. Add the rinsings to the absorbers, and titrate as directed in Section 11.
