The physical, chemical, and thermal changes in fabrics treated with a commercial crease-resisting compound (CPNS) were investigated. The samples were analyzed by a scanning electron microscope equipped with an energy dispersive X-ray microanalyzer, elemental analysis, and differential thermogravimetry. X-ray microanalysis of the treated fabrics revealed that changes in gross integral counts of O, N, Mg, Al, Si, S, Cl, and Ca as a result of the treatments were related to the application rate of the compound. This result was broadly supported by mineral analysis data determined by standard wet chemistry methods. The effects of over- and undercuring were also investigated. in addition, the increase in nitrogen content as a result of the higher application rate can also be detected by EA. Differential thermogravimetric analyses of the samples showed distinct changes in the profile of the thermally stable fraction. This could be due to the formation of a crosslinked cellulose complex, which pyrolyzed at the significantly higher decomposition temperature of 481 degrees C in comparison with 473 degrees C for untreated material. The advantages of using instrumental techniques for assessing the efficiency of treatments are briefly discussed.