建立了微波消解前处理,全反射X射线荧光法(TXRF)同时测定松花粉中K、Ca、Ti、Mn、Fe、Ni、Cu、Zn和Rb9种生命元素含量的分析方法.松花粉原料经过微波消解前处理后,采用全反射X射线荧光光谱净计数、QXAS分析软件解谱和单一内标法进行定量分析.比较了干灰化法、湿消解法和微波消解法3种前处理方法的效果,并确立微波消解法作为样品前处理方法.用微波消解- TXRF法测定了花粉标准物质中的上述9种元素,并计算得到其仪器检出限(LLD)为0.002～0.054 mg/L,方法检出限(LDM)为0.004～0.122 mg/kg.TXRF法测定各元素的相对标准偏差(RSDs)为1.0％～5.5％.该方法操作简单、样品用量少、检出限低,对实际样品松花粉的测定结果与ICP - MS法无显著性差异.%A method for the determination of nine life elements ( K, Ca, Ti, Mn, Fe, Ni, Cu, Zn and Rb) in pine pollen was developed by microwave digestion and total reflection X-ray fluorescence (TXRF). The pollen was digested by microwave digestion. The counts, QXAS software and internal standard method were used for TXRF measurement. Effects of three sample preparation methods including dry ashing method, wet nitration method and microwave digestion method, on the TXRF results of certified reference material (GBW10026) were compared. The microwave digestion method was selected as the pretreatment method. Nine elements in GBW10026 were determined by TXRF with microwave digestion. The lower limit of detection ( LLD) and the limit of determination (LDM) for different elements in pollen were calculated to be 0.002 -0.054 mg/L and 0.004 -0. 122 mg/kg, respectively. The relative standard deviations ( RSDs) were lower than 5. 5% . This method showed advantages of easy operation, less sample consumption and low detection limit. The method was used to analyse the content of 9 elements in pine pollen, and there were was no significant difference between the results and those of ICP - MS.
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