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    超级微波消解-电感耦合等离子体质谱法测定三聚磷酸铝中15种微量元素

    Determination of 15 Trace Elements in Aluminum Tripolyphosphate by Inductively Coupled Plasma Mass Spectrometry with Super Microwave Digestion

    • 摘要: 随着行业要求和环保法规的完善,对化工产品三聚磷酸铝(ATP)中有毒有害重金属元素含量的要求越来越严格,而相关检测标准未见报道,因此提出了用于测定ATP中铬、锰、铁、钴、镍、铜、锌、砷、镉、锑、钡、汞、铊、铅和铋共15种元素含量的题示方法。样品于105 ℃预干燥3 h后,分取0.100 0 g,加入3 mL硝酸和3 mL磷酸,将混合物置于超级微波消解仪中,程序升温至240 ℃消解30 min。冷却至室温,用水将消解液稀释至50 mL,采用电感耦合等离子体质谱法测定,并通过在线引入锗、铟、铼内标混合液、碰撞反应池技术以及动能歧视(KED)技术消除质谱干扰和非质谱干扰。结果显示:各元素的质量浓度在一定范围内和对应的信号响应值与内标信号响应值的比值呈线性关系,检出限(3s)为0.000 300~0.421 mg·kg−1;按照标准加入法进行回收试验,回收率为82.1%~110%,测定值的相对标准偏差(n=6)均小于6.0%。

       

      Abstract: With the improvement of industry requirements and environmental regulations, the requirements for the content of toxic and harmful heavy metal elements in chemical products of aluminum tripolyphosphate (ATP) are becoming increasingly strict. However, there have been no reports on relevant testing standards. Therefore, the method mentioned by the title was proposed to determine the content of 15 elements including chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, cadmium, antimony, barium, mercury, thallium, lead, and bismuth in ATP. After pre-drying the sample at 105 ℃ for 3 h, an aliquot (0.100 0 g) was taken, and 3 mL of nitric acid and 3 mL of phosphoric acid were added. The mixture was placed in a super microwave digestion apparatus and digested at 240 ℃ for 30 min by heating program. After cooling to room temperature, the digestion solution was diluted to 50 mL by water, and determined by inductively coupled plasma mass spectrometry. Introduction of a mixture of germanium, indium, and rhenium internal standards online, collision reaction cell technology and KED technology was used to eliminate mass spectrometry interference and non-mass spectrometry interference. It was shown that linear relationships between values of the mass concentration and corresponding signal response ratio of each element to internal standard were kept in definite ranges, with detection limits (3s) in the range of 0.000 300-0.421 mg·kg−1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 82.1%-110%, and RSDs (n=6) of the determined values were less than 6.0%.

       

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