Abstract: GC-MS was applied to the determination of p-chloroaniline in textiles. Stability of p-chloroaniline solution was studied and it was found that the standard solution and sample solution were stable at high concentrations (e.g., 30 mg·L-1) and low temperatures (e.g., <5 ℃). Under the optimized conditions, tests for recovery and precision were made by standard addition method at 3 different concentration levels of 10.0, 20.0, 30.0 mg·kg-1, values of recovery found were 86.0%, 100.6% and 97.6% respectively, and values of RSD′s (n=6) was less than 9.0%.