The internal standard method coupled with the standard addition method has been applied to the analysis of environmental materials, such as urban particulate matter, vehicle exhaust particulates and coal fly ash by photon activation. High-resolution gamma-ray spectrometry makes possible to use multi-internal standard gamma-rays, in order to crosscheck the analytical results obtained from each internal standard. It was ascertained that this method can provide not only accurate analytical results but also the information of homogeneity of samples, correlation of elements in the sample, loss or contamination in the preparation process.