Luminescence dating is widely applied nowadays, mainly for archaeological material and artefacts and sediments of all types and origins. However, optically stimulated luminescence (OSL) from archaeological sediment, originated from mud brick buildings has been hardly studied. The archaeological sites of Tall Abu Fahd and Tall Qsubi are located in the Middle Euphrates Valley, Deir ez-Zor district, Syria. These two Bronze Age sites were recently discovered by a Spanish-Syrian team from the Directorate General of Antiquities and Museums (Damascus) and the University of Coruña. Both sites were dated (about 3.5 ka BC) by typological pottery classification. Sediment and pottery samples from these archaeological sites were collected for luminescence dating. Several analytical procedures for obtaining equivalent doses were tested on the sediment samples. Blue OSL from quartz subsamples and IRSL, post IRSL Blue OSL from feldspar contaminated quartz and polymineral subsamples were performed to obtain OSL ages. For the pottery samples, additive dose TL on a coarse grain feldspar contaminated quartz subsample was performed as well. Results have shown agreement among all the luminescence procedures tested on the Tall Abu Fahd site samples after fading correction, showing ages around 2.7 ka BP. Obtained ages from the other site samples show disagreement among quartz blue OSL and the other subsamples. Fading ratios allow correcting age underestimations from the polymineral post-IR OSL signal. However, the polymineral IRSL signal still shows underestimation. Final sediment and pottery ages have shown good agreement. Older ¹⁴C independent age (3.32 ka BP) corresponds to occupational periods of the site while sediment ages are attributed to a post occupation phase.