D5453_11 (16e1)

Obtain a test specimen using the procedure described in Section 8 of the written standard. The sulfur concentration in the test specimen must be less than the concentration of the highest standard and greater than the concentration of the lowest standard used in the calibration. If required, a dilution can be performed on either a weight or volume basis. Record the mass of the test specimen and the total mass of the test specimen and solvent. Record the mass of the test specimen and the total volume of the test specimen and solvent. Measure the response for the test specimen solution using one of the procedures described in 10.2 through 10.4 of the written standard. Inspect the combustion tube and other flow path components to verify complete oxidation of the test specimen. Reduce the sample size or the rate of injection, or both, of the specimen into the furnace if coke or sooting is observed. Increase the residence time for the boat in the furnace if coke or soot is observed on the boat. Decrease the boat drive introduction rate or specimen sample size, or both, if coke or soot is observed on the exit end of the combustion tube. Clean any coked or sooted parts per manufacturer's instructions. After any cleaning or adjustment, assemble and leak check the apparatus. Repeat instrument calibration prior to re-analysis of the test specimen. To obtain one result, measure each test specimen solution three times and calculate the average detector responses. Density values needed for calculations are to be measured using Test Methods D1298, D4052, or equivalent, at the temperature at which the sample was tested.