A reproducible method for determination of nitrocellulose in soil.

ABSTRACT

A reproducible analytical method for determination of nitrocellulose in soil is described. The new method provides the precision and accuracy needed for quantitation of nitrocellulose in soils to enable worker safety on contaminated sites. The method utilizes water and ethanol washes to remove co-contaminants, acetone extraction of nitrocellulose, and base hydrolysis of the extract to reduce nitrate groups. The hydrolysate is then neutralized and analyzed by ion chromatography for determination of free nitrate and nitrite. A variety of bases for hydrolysis and acids for neutralization were evaluated, with 5N sodium hydroxide and carbon dioxide giving the most complete hydrolysis and interference-free neutralization, respectively. The concentration of nitrocellulose in the soil is calculated from the concentrations of nitrate and nitrite and the weight percentage of nitrogen content in nitrocellulose. The laboratory detection limit for the analysis is 10mg/kg. The method acceptance range for recovery of nitrocellulose from control samples is 78-105%.