ASTM D3606 Standard Test Method for Determination of Benzene and Toluene
ASTM D3606 Standard Test Method for Determination of Benzene and Toluene in Finished Motor and Aviation Gasoline by Gas Chromatography
8. Preparation of Column Packings
8.1 Prepare two packing materials (one packing material consists of 10 mass % dimethylpolysiloxane on Chromosorb W; the other, 20 mass % TCEP on Chromosorb P) in accordance with the following procedures:
8.1.1 Dimethylpolysiloxane Packing - Weigh 45 g of the Chromosorb W, 60 to 80 mesh and pour into the 500-mL flask (5.10). Dissolve 5 g of the dimethylpolysiloxane in approximately 50 mL of chloroform. (Warning - See Note 3.) Pour the methyl silicone-chloroform solution into the flask containing the Chromosorb W. Attach the flask to the evaporator (5.9), connect the vacuum, and start the motor. Turn on the infrared lamp and allow the packing to mix thoroughly until dry.
8.1.2 1,2,3-Tris(2-cyanoethoxy)Propane(TCEP) Packing - Weigh 80 g of Chromosorb P, 80 to 100 mesh and pour into the 500-mL flask (5.10). Dissolve 20 g of TCEP in 200 mL of methanol and pour into the flask containing the Chromosorb P. Attach the flask to the evaporator (5.9), connect the vacuum, and start the motor. Turn on the infrared lamp and allow the packing to mix thoroughly until dry. (Do not heat the packing over 180°C.)
9. Preparation of Column
9.1 Cleaning Column - Clean the stainless steel tubing as follows. Attach a metal funnel to one end of the steel tubing. Hold or mount the stainless steel tubing in an upright position and place a drain beaker under the outlet end of the tubing. Pour about 50 mL of methylene chloride (Warning - See Note 4) into the funnel and allow it to drain through the steel tubing and into the drain beaker. Repeat the washing procedure with 50 mL of acetone. (Warning - See Note 5) Remove the funnel and attach the steel tubing to an air line, using vinyl tubing to make the connection. Remove all solvent from the steel tubing by blowing filtered, oil-free air through or pulling a vacuum.
9.2 Packing Columns - Preform Columns A and B separately to fit the chromatograph. Pack the 0.8-m tubing (Column A) with the dimethylpolysiloxane packing (8.1.1) and the 4.6-m tubing (Column B) with the TCEP packing (8.1.2) using the following procedure. Close one end of each tubing with a small, glass wool plug, and connect this end to a vacuum source by means of a glass wool-packed tube. To the other end connect a small polyethylene funnel by means of a short length of vinyl tubing. Start the vacuum and pour the appropriate packing into the funnel until the column is full. While filling each column, vibrate the column with the electric vibrator to settle the packing. Remove the funnel and shut off the vacuum source. Remove the top 6 mm (1/4-in.) of packing and insert a glass wool plug in this end of the column.
