Optimization of supercritical fluid derivatization and extraction of cresols in soil samples using factorial designs

✍ Scribed by Maria P. Llompart; Rosa A. Lorenzo; Rafael Cela

• Publisher: John Wiley and Sons
• Year: 1996
• Tongue: English
• Weight: 968 KB
• Volume: 8
• Category: Article
• ISSN: 1040-7685
• DOI: 10.1002/(sici)1520-667x(1996)8:3<163::aid-mcs1>3.0.co;2-#

✦ Synopsis

Two-and three-factorial designs have been used to optimize the supercritical fluid acetylation-extraction of o-cresol, m-cresol and p-cresol in soil samples. Overall, nine variables (carbon dioxide flow rate, fluid density, extraction cell temperature, static extraction time, nozzle and trap temperatures, amount of derivatizing reagent, amount of pyridine, and contact time between the derivatizing reagents and the sample) were considered. The results suggest that only extraction cell temperature and the amount of derivatizing reagent are statistically significant to the overall extraction yield, as is the extractant flow rate to the kinetics. Special attention was paid to developing suitable test materials for these types of optimization processes. The procedure was validated by processing a certified reference material.