||A screening procedure was developed for the determination of the targeted 49 priority pollutants in soil. An extraction procedure followed by capillary GC-MS analysis was used. Dual pH solutions with methylene chloride were used as extraction solvent system. Both base/neutral and acidic fractions were analyzed on the same fused silica 30 meter SPB-1 (SE-30) column. A GC-FID with a 60 meter wide-bore SPB-1 glass capillary column was used for quantitative analysis due to its larger sample capacity and higher sensitivity. The precision and accuracy for 5.1 ppm (51 (mu)g/10 g) concentration in "zero soil" is less than 25% RSD. A headspace technique was also developed for the determination of volatile compounds from the 49 priority pollutants in soil. The same instrumental conditions and columns were used as in the extraction procedure. The headspace sample preparation used a 20 mL glass vial containing 3 grams soil with 10 mL pH 13 spiked solution equilibrated at 30(DEGREES)C for one hour before 0.5 mL headspace is withdraw and injected into the gas chromatograph. A reference system was also set up by using 3 grams sand in 10 mL pH 13 spiked solution for the study of the efficiency of the soil headspace analysis. Once the recovery rate between the soil and the reference system was established, the ratio can be used for the determination of other soil samples from the same origin. The precision and accuracy for 3 grams soil sample spiked with 5.1 ppm (51 (mu)g/ 10 mL) pollutant mixture in a 20 mL vial is less than 3% RSD.