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作 者:王小平 刘淑萍 赵丹 WANG Xiaoping;LIU Shuping;ZHAO Dan(Gansu Institute of Metrology,Lanzhou 730000,China)
机构地区:[1]甘肃省计量研究院,兰州730000
出 处:《化学分析计量》2025年第3期51-55,62,共6页Chemical Analysis And Meterage
基 金:甘肃省市场监督管理局科技计划项目(SSCJG-BJ-201902)。
摘 要:建立了微波消解-原子荧光光谱法测定百合中砷含量。采用高温高压密闭消解罐消解百合样品,避免了易挥发元素砷的损失。采用原子荧光光度计测定,灯电流为40 mA,负高压为280 V,原子化温度为200℃,载气流量为300 mL/min。砷元素的质量分数在0.1~2.0μg/kg范围内与光谱强度线性关系良好,相关系数为0.9999,检出限为0.0042μg/kg。精密度试验测定结果的相对标准偏差为1.79%(n=6)。3种不同浓度加标水平下,平均回收率为96.5%~102%。该方法操作简便、快速、灵敏度高,经国家一级标准物质GBW 10022验证和样品加标回收试验,结果显示该方法准确可靠。A method for the determination of arsenic in Lily Bulb by microwave digestion atomic fluorescence spectrometry was established.The loss of volatile element arsenic was avoided by using high temperature and high pressure closed digestion tank to digest lily samples.The lamp current was 40 mA,the negative high voltage was 280 V,the atomization temperature was 200℃,and the carrier gas flow rate was 300 mL/min.The mass fraction of arsenic had a good linear relationship with the spectral intensity in the range of 0.1-2.0μg/kg,the correlation coefficient was 0.9999,and the detection limit was 0.0042μg/kg.The relative standard deviation of the precision test results was 1.79%(n=6).The average recovery rate was 96.5%-102%at three different concentration levels of spiked samples.The method is simple,rapid and sensitive,and it has been verified by the national standard material GBW 10022 and the sample recovery rate test.The results show that the method is accurate and reliable.
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