ASTM D5480 Standard Test Method for Engine Oil Volatility by Gas chromatography
5. Apparatus
5.1 Chromatograph, any gas chromatograph can be used that has the following characteristics:
5.1.1 Oven, a column oven having high-temperature (400°C/752°F) capability is required.
5.1.2 Detector, a flame ionization detector capable of continuous operation at temperatures of 405°C (761°F) is required.
5.1.3 Column Temperature Programmer - The chromatograph must be capable of reproducible linear temperature programming over the temperature range required for the test method.
5.1.4 Sample inlet System - The sample inlet system must provide for on-column injection or equivalent such as programmable splitless injection.
5.1.5 Column, 12 m by 0.53 mm by 0.15 μm nonpolar carborane modified polydimethylsiloxane bonded phase column or equivalent that can withstand the high column oven temperature employed, and meets the resolution requirements stipulated in 7.3 must be used.
5.1.6 Integrator - Means must be provided for determining the accumulated area under the chromatogram. This can be done by means of a computer or electronic integrator. A timing device can be used to record the area at set time intervals. The same basis for measuring time must be used to determine the retention times of the internal standard components and the tetracosane. The maximum signal measured must be within the linear range of the measuring system used.
5.1.7 Pressure/Flow Controller - the chromatograph must be equipped with a constant pressure/constant flow device capable of maintaining the carrier gas at a constant flow rate throughout the temperature program.
5.1.8 Microsyringe, required for the introduction of sample to the gas chromatograph. A 10-μl syringe is recommended.
6. Reagents and Materials
6.1 Purity of Reagents - Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of suficiently high purity to permit its use without lessening the accuracy of the determination.
6.2 Carbon Disulfide (CS2)
NOTE 1: Warning - Carbon disulfide is extremely flammable. Also, breathing of its vapor and skin contact should be avoided.
6.3 Carrier Gas - Helium (high purity). Additional purfication is recommended by the use of molecular sieves or other suitable agents to remove water, oxygen, and hydrocarbons.
NOTE 2: Warning - Helium is a compressed gas under high pressure.
6.4 Detector Gases - Air, hydrogen
NOTE 3: Warning - Air and hydrogen are compressed gases under high pressure Hydrogen is an extremely Flammable gas.
6.5 Decane [CH3(CH2)8CH3]
6.6 Dodecane [CH3(CH2)10CH3]
6.7 Hexadecane[CH3(CH2)14CH3]
6.8 Octadecane [CH3(CH2)16CH3]
6.9 Tetracosane [CH3(CH2)22CH3]
6.10 Undecane [CH3(CH2)9CH3]
