离子色谱法测定核电站一回路冷却剂中痕量F~-,Cl~-和SO_4~(2-)
|
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.
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
[1]白新德.核材料化学[M].北京:化学工业出版社,2007:391–466.
[2]韩延德.核电厂水化学[M].北京:原子能出版社,2010:30–42.
[3]牟世芬,刘克纳,丁晓静.离子色谱方法及应用[M].北京:化学工业出版社,2005:1–5.
[4]鲁蕴甜.离子色谱在环境分析中应用概述[J].广东化工,2014,41(11):166–167.
[5]潘灿盛,李维嘉,吴凌涛,等.离子色谱在饮用水及食品分析中的应用研究[J].广州化工,2014,42(7):33–34,95.
[6]宋利君,刘飞华,李成涛,等.B–Li水化学对核电站金属材料腐蚀的影响[J].核科学与工程,2014,34(1):97–101,115.
[7]蔡艳艳,于军波,马艳,等.离子色谱技术的发展及其在食品添加剂检测中的应用[J].分析仪器,2013(6):1–6.
[8]李昌厚.高效液相色谱研发和应用中关键问题的研究[J].分析仪器,2013(3):44–49.
[9]张燕,韩秉均,唐新建,等.火电机组水汽中痕量阴离子的毛细管离子色谱法测定[J].热力发电,2015(9):19–25.
[10]余秀娟,曾钰,那晶晶,等.离子色谱法同时测定水中8种阴离子[J].环保科技,2015(4):57–59.
[11]蒋晓光,王艳君,王彩云,等.硫代硫酸钠滴定法连续测定铜磁铁矿中铜和铁[J].化学分析计量,2015,24(3):22–26.
[12]曾兴宇,刘静,周东星.紫外消解流动注射光度法测定海水养殖废水中总氮、总磷[J].化学分析计量,2015,24(3):62–65.
[13]HJ 168–2010环境监测分析方法标准制修订技术导则[S].
[2]韩延德.核电厂水化学[M].北京:原子能出版社,2010:30–42.
[3]牟世芬,刘克纳,丁晓静.离子色谱方法及应用[M].北京:化学工业出版社,2005:1–5.
[4]鲁蕴甜.离子色谱在环境分析中应用概述[J].广东化工,2014,41(11):166–167.
[5]潘灿盛,李维嘉,吴凌涛,等.离子色谱在饮用水及食品分析中的应用研究[J].广州化工,2014,42(7):33–34,95.
[6]宋利君,刘飞华,李成涛,等.B–Li水化学对核电站金属材料腐蚀的影响[J].核科学与工程,2014,34(1):97–101,115.
[7]蔡艳艳,于军波,马艳,等.离子色谱技术的发展及其在食品添加剂检测中的应用[J].分析仪器,2013(6):1–6.
[8]李昌厚.高效液相色谱研发和应用中关键问题的研究[J].分析仪器,2013(3):44–49.
[9]张燕,韩秉均,唐新建,等.火电机组水汽中痕量阴离子的毛细管离子色谱法测定[J].热力发电,2015(9):19–25.
[10]余秀娟,曾钰,那晶晶,等.离子色谱法同时测定水中8种阴离子[J].环保科技,2015(4):57–59.
[11]蒋晓光,王艳君,王彩云,等.硫代硫酸钠滴定法连续测定铜磁铁矿中铜和铁[J].化学分析计量,2015,24(3):22–26.
[12]曾兴宇,刘静,周东星.紫外消解流动注射光度法测定海水养殖废水中总氮、总磷[J].化学分析计量,2015,24(3):62–65.
[13]HJ 168–2010环境监测分析方法标准制修订技术导则[S].