Summary: In 1994, in tbe first comprehensive Investigation of persistent organochlorine contaminants in a country of the former Soviet Union, we measured congener-specific levels of polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), and polychtorinated dibenzofurans (PCDFs), as well as 19 organochlorine pesticides (OC) in breast milk samples collected using the WHO protocol from first-time mothers ('primiparae') living in southern Kazakhstan. High levels (up to 80 pg/g fat) of 2,3,7,S-tetrachlorodibenzo-p-dioxin (TCDD) were found in breast milk samples from villages in a cotton-growing region in soutbern Kazakhstan, with TCDD contributing 70-80% of tbe I-TEQ. In these samples, the I-TEQ arose almost exclusively from two congeners, TCDD and the pentachlorodibenzo-p-dioxin (PeCDD). A follow-up study in 1997 measured levels of PCDDs/PCDFs in samples from the region's cotton-growing State Farms. As part of our continuing characterization of this TCDD contamination, we investigated the effectiveness of the CALUX™ assay to screen and identify breast milk samples with high contaminant levels. We report the results of correlation studies on CALUX™ and GC/MS/MS data using these samples, where two dioxin congeners are responsible for most of the I-TEQ.