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In the present work,a new apparatus of diaphragm glow discharge emission spectroscopy was described for the determination of potassium and sodium ions in aqueous solution.The discharge was formed in a pin hole on a dielectric diaphragm interposed between two submerged graphite electrodes.Effects of pH and applied voltage on the determination have been examined.It was found that decreasing the solution pH and increasing the applied voltage were favorable for the determination performance.Limits of detection for Na and K were 0.002 and 0.05mg L-1under the optimum conditions,respectively.It demonstrates that the diaphragm glow discharge emission spectroscopy is a promising technique in measurements of metal ions in aqueous solution,because no optical interferences from the electrodes were found.