D5453_19_11

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 resident's 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 3 times, and calculate the average detector responses. Determine density values, gram and milliliter needed for calculations, by performing a gravimetric weighing of the test sample into a Class-A volumetric flask. See, Note 14: C-Section 12.1. During the various inter-laboratory studies, see, 15.1:Test Sample Density Values. Gram and milliliter needed for calculations are always provided to participants, and were determined by the ILS distributor in a variety of ways, including information supplied by bulk sample suppliers. Accompanying information from documentations, such as safety data sheets, and gravimetric weighing into a volumetric flask at ambient laboratory temperatures, with the gravimetric method being the most common. Density values needed for calculations, may be measured using test methods: D-1298 and D-4052 or equivalent. See, Note 15. Users of the test method, may convert density measured at standard temperature, to the temperature at which the sample was tested, by using Guide D-1250 and its adjuncts.