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微波消解样品-石墨炉原子吸收光谱法测定豆制品中铅 被引量:4

GF-AAS Determination of Lead in Bean Products with Microwave Assisted Sample Digestion
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摘要 豆制品试样置于微波消解罐中用硝酸及过氧化氢在MDS-2002A型微波消解仪中消解,所得试样的稀硝酸溶液,在加入硝酸铵后直接进样作石墨炉原子吸收光谱法测定。硝酸铵的加入除作为基体改进剂外,还能起提高灰化温度和消除氯化钠干扰的作用。对仪器的工作条件,特别是石墨炉工作程序的参数,包括烘干时间、灰化及原子化温度等进行了试验并予以优化。所选用的分析谱线的波长为283.3nm,在所测得的峰高积分值与铅的质量浓度在2~80μg·L^(-1)范围内呈线性关系。方法的检出限(S/N=3)为0.1μg·L^(-1)。以豆制品样品为基体加入铅标准溶液做方法的回收试验,测得回收率在94.0%~102.0%之间。 Bean product sample was digested with HNO3 and H2O2 in the MDS-2002A microwave digestor under prescribed conditions, and the solution in dil. HNO3 was used directly for GF-AAS determination. Ammonium nitrate was added to the sample solution as matrix modifier, and to elevate the ashing temperature as well as to eliminate interference from sodium chloride. Working conditions of the instrument, especially the parameters of working program of the graphite furnace, including time of drying, temperature for ashing and atomization etc. , were studied and optimized. Linear relationship between values of integration of peak heights and concentration of Pb^2+ ion was obtained in the range of 2-80 μg · L^-1 , with detection limit (S/N=3) of 0. 1 μg · L^-1. The wavelength of analytical spectral line selected was 283. 3 nm. Test for recovery was made by standard addition method, and the results obtained were in the range of 94. 0%-102. 0%.
作者 岳志坚
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2008年第9期826-827,共2页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 石墨炉原子吸收光谱法 微波加热消解试样 铅离子 豆制品 GF-AAS Microwave assisted sample digestion Lead ion Bean products
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  • 1GB/T5009.12-2003.食品中铅的测定[S].[S].,..

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