建立了自动电位滴定仪测定工业用氢氧化钠中氢氧化钠及碳酸钠的方法,对滴定模式、主要滴定参数及等当点的判断进行了选择试验,选择在自动电位滴定仪动态滴定模式下,优化主要的滴定参数为最小增量体积为30 μL、测量点密度为4、信号漂移判据为50 mV/min,以pH 8～9和pH 5左右的等当点判断为本方法的真实正确的等当点.用自动电位滴定仪代替手工滴定操作,测定工业用氢氧化钠中氢氧化钠及碳酸钠的结果与国家标准方法和双指示剂法相吻合,氢氧化钠和碳酸钠相对标准偏差(n=5)分别为0.03%～0.05%、0.74%～0.90%;碳酸钠的回收率为99.0%～100.5%.
An automatic potentiometric titration method was established for the determination of sodi-um hydroxide and sodium carbonate in industrial sodium hydroxide. The titration mode, main titra-tion parameters and the judgment of equivalent point were tested and selected. Under the dynamic ti-tration mode of automatic potentiometric titrator, the optimized main titration parameters were. mini-mum increasing volume of 30 μL, measurement point density of 4 and signal shift criterion of 50 mV/min. The equivalent points at pH 8-9 and pH 5 were used to evaluate the trueness of this method. The manual titration operation was replaced by automatic potentiometric titrator. The determination re-suits of sodium hydroxide and sodium carbonate in industrial sodium hydroxide were consistent with the GB method and dual-indicator method. The relative standard deviations (RSD, n=5) for sodium hydroxide and sodium carbonate were 0.03 %-0.05 % and 0.74 % ～0. 90 %, respectively. The re-covery rate of sodium carbonate was 99.0 %-100.5%.
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