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This study was carried out to determine serum electrolytes levels in kidney failure subjects undergoing dialysis in Owerri. Sixty (60) subjects between the age of eighteen and seventy years were selected for the study. Sodium & Potassium were determined by Emission Flame Photometry and Chloride was determined by Mercuric Nitrate method. The test was calculated statistically to get the means. P<0.05 was considered statistically significant while P>0.05 was considered not statistically significant. The levels of these ions were correlated. Sodium ion concentration was statistically and significantly decreased (p=0.001) in kidney failure subjects undergoing dialysis when compared with the control subjects. There was statistical significant difference (p=0.000) in the mean value of potassium ion concentration in kidney failure subjects undergoing dialysis when compared with the control subjects. There was statistical significant difference (p=0.001) in the mean value of chloride ion concentration in kidney failure subjects undergoing dialysis when compared with the control subjects. There was statistical significant difference (p=0.000) in the mean value of bicarbonate ion in kidney failure subjects undergoing dialysis when compared with the control subjects. There was a significant negative correlation of sodium ion with potassium and bicarbonate ion (r= -0.107, p=0.000; r=-0.192, p=0.000 respectively which indicates an increase in sodium with decrease in potassium and bicarbonate. There was a significant positive correlation of sodium ion with chloride ion (r=-0.185, p=0.000) which indicates increase in sodium leading to increase in chloride. There was a significant negative correlation of potassium ion with chloride (r= -0.130, p=0.000) which indicates increase in potassium leading to a decrease in chloride. There was a significant positive correlation of potassium ion with bicarbonate ion (r=-0.760, p=0.000) which indicates increase in potassium leading to increase in bicarbonate. There was significantly no correlation between chloride ion with bicarbonate ion (r=-0, p=0.000). Sodium, Chloride and Bicarbonate ion concentrations were statistically and significantly increased in kidney failure subjects undergoing dialysis when compared with the control subjects indicating hypernatremia and hyperchloremia and alkalosis respectively while Potassium ion concentrations was decreased indicating hypokalemia. The use of dialysis is effective in balancing the levels of these ions that were abnormally low and high respectively in Kidney failure subjects.