In the proposed work an ultrasound assisted ion pair based surfactant-enhanced dispersive liquid-liquid microextraction (UA-IPSE-DLLME) with solidification of floating organic drop was studied for preconcentration and flame atomic absorption spectrometry (FAAS) determination of nickel and cobalt ions in vegetable and herb samples. Congo Red (CR) and didecyldimethyl ammonium chloride (DDMAC) were used as complexing and ionpairing agents, respectively. By using ion-pairing agent CR-metal complexes gained more hydrophobic character and extracted into 1-dodecanol more efficiently. Some parameters affect extraction efficiency were studied and some analytical characteristics of the method were calculated. Under optimized conditions, detection limit of 1.7 mu g L-1 and 2.4 mu g L-1, quantification limit of 5.6 mu g L-1 and 7.9 mu g L-1 and enrichment factors of 65 and 48 were obtained for nickel and cobalt, respectively. Relative standard deviation (n= 7) for 100 mu g L-1 nickel and cobalt were 3.6% and 3.8%, respectively. The proposed UA-IPSE-DLLME method has been successfully applied for the determination of nickel and cobalt ions in certified reference materials and some food samples.