摘要
建立离子色谱法测定核电站一回路冷却剂中痕量氟离子F~-,氯离子Cl~-,硫酸根离子SO_4~(2-)的方法。采用80 mmol/L硼酸溶液配合氢氧化钾淋洗液发生器在线生成淋洗液,梯度洗脱,淋洗液流量为1.2 mL/min,在选定的分析条件下,NO_2~-,NO_3~-,PO_4~(3-)和CO_3~(2-)不干扰F~-,Cl~-,SO_4~(2-)的测定。F~-,Cl~-,SO_4~(2-)的质量浓度与其色谱峰面积呈良好的线性关系,线性相关系数分别为0.999 8,0.999 5,0.999 7,线性范围分别为0.85~30.0,2.65~30.0,2.00~30.0μg/L。F~-,Cl~-,SO_4~(2-)测定结果的相对标准偏差分别为0.56%~1.58%,0.85%~3.62%,1.21%~4.60%(n=7)。F~-,Cl~-,SO_4~(2-)的加标回收率分别为98%~104%,98%~108%,93%~108%。该方法快速、准确,满足核电站一回路冷却剂中痕量F~-,Cl~-,SO_4~(2-)的检测要求。
The method was established for determination of trace F~-,Cl~- and SO_4~(2-) in power plant primary coolant by ion chromatography. The 80 mmol/L boric acid was coordinated with the KOH eluent generator to produce new eluent online for gradient elution,and eluent flow rate was 1.2 mL/min. Under the selected conditions,the determination of F~-,Cl~- and SO_4~(2-) were not influenced by NO_2~-,NO_3~-,PO_4~(3-) and CO_3~(2-). The mass concentration of F~-,Cl~- and SO_4~(2-) were linear with its peak areas. The correlation coefficients of F~-,Cl~-, SO_4~(2-) were 0.999 8, 0.999 5, 0.999 7, and the detection limits were 0.85-30.0,2.65-30.0,2.00-30.0 μg/L, respectively. The relative standard deviations of F~-,Cl~-, SO_4~(2-) detection results were 0.56%-1.58%,0.85%-3.62%, 1.21%-4.60%(n=7), respectively. The recoveries of F~-,Cl~- and SO_4~(2-) were 98%-104%,98%-108%, 93%-108%, respectively. The method can be used for detecting trace F~-,Cl~-, SO_4~(2-) in power plant primary coolant quickly and accurately.
引文
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