石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙
刘晓军1,罗坤1,郑德超1,陈思羽2,杨博文2,彭木林1,赵红杰1,叶伟1
1. 广西防城港核电有限公司,广西防城港 538000; 2. 中核深圳凯利核能服务有限公司防城港分公司,广西防城港 538000
Determination of calcium in boric acid medium of pressurized water reactor by graphite furnace atomic absorption spectrometry
刘晓军1,罗坤1,郑德超1,陈思羽2,杨博文2,彭木林1,赵红杰1,叶伟1
1. Guangxi Fangchenggang Nuclear Power Co., Ltd., Fangchenggang 538000, China; 2. Fangchenggang Branch, CNNC Shenzhen KaiLi Nuclear Power Service Co., Ltd., Fangchenggang 538000, China
摘要:以甘露醇为基体改进剂,建立石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙含量的方法。考察基体改进剂用量、灰化温度、原子化温度、基体干扰以及共存离子干扰对测定结果的影响,确定最佳测定条件:以硼含量为1 000 mg/kg 的硼酸为背景基体,加入适量甘露醇,样品作酸化处理,灰化温度为1 700℃,原子化温度为2 450℃。钙含量在8~32 μg/kg 范围内与光谱强度成良好的线性关系,相关系数为0.999 6,方法检出限为1.79 μg/kg。对于硼基体含量为0~2 500 mg/kg 的样品,测定结果的相对标准偏差为0.5%~7.5%(n=6),相对误差不大于13.2%,加标回收率为93.9%~113.3%。该方法检测速度快,结果准确,能满足实际生产要求。
Abstract:The method for determination of calcium in boric acid medium of pressurized water reactor by graphite
furnace atomic absorption spectrometry with mannitol as matrix modifier was established. The effects of the amount of
matrix modifier, ashing temperature, atomization temperature, matrix interference and co-existent element interference
on the determination resutls were investigated. The optimum determination conditions were determined: boric acid with
boron content of 1 000 mg/kg was used as the background matrix, adding appropriate mannitol, the sample was acidified,
the ashing temperature was 1 700 ℃, and the atomization temperature was 2 450 ℃. The content of calcium had a good
linear relationship with the spectral intensity in the range of 8-32 μg/kg, the correlation coefficient was 0.999 6, and the
detection limit of the method was 1.79 μg/kg. For the samples with boron matrix content of 0-2 500 mg/kg, the relative
standard deviations of determination results were 0.5%-7.5% (n=6), the relative error were not more than 13.2%, and the
standard addition recovery was 93.9%-113.3%. The method is rapid and accurate, which can satisfy the actual production
requirements.
关键词:甘露醇;石墨炉原子吸收光谱法;硼酸;钙
Keywords:mannitol; graphite furnace atomic absorption spectrometry; boric acid; calcium
本文引用格式:
刘晓军,罗坤,郑德超,等. 石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙[J]. 化学分析计量,2020,29(2):71-74.
LIU X J,LUO K,ZHENG D C,et al. Determination of calcium in boric acid medium of pressurized water reactor by graphite furnace atomic absorption spectrometry[J]. Chemical analysis and meterage,2020,29(2):71-74.
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