Traces of toxic metals such as chromium and copper are common in some varieties of Portland cement and as such cause pollution and are harmful to human beings and other living systems. Both acidulation and dry fusion lithium metaborate methods have been investigated; the latter has been developed for determination of chromium and copper using electrothermal atomization. Instrument settings and analytical parameters have been optimized and determined for each metal. The samples analyzed were collected from two main factories, Falluja and Kuffa Portland cement factories, about 250 km apart. Samples from Falluja contained 123.2 ppm chromium and no copper, whereas those from Kuffa contained 117.6 and 80.8 ppm chromium and copper, respectively. When standard Portland cement is used for matrix matching of standard solutions of chromium and copper, no matrix interference is observed and the analyte addition technique is not required.