电感耦合等离子体质谱法测定谷物样品中 铝的样品处理方法研究

Pre-treatment of the determination of aluminum in the grain samples by inductively coupled plasma mass spectrometry

中文关键词:  电感耦合等离子体质谱法  铝  谷物  前处理

英文关键词:inductively coupled plasma mass spectrometry (ICP-MS)  aluminum  grain  pre-treatment methods

中文摘要:

      目的 建立电感耦合等离子体质谱法(ICP-MS)测定谷物样品中铝的准确分析方法。方法 本文研究了4种样品前处理方法: 干灰化法、微波消解(硝酸-双氧水体系)、微波消解(硝酸-氢氟酸-双氧水体系)、微波消解(硝酸-氢氟酸-双氧水体系消解, 加高氯酸二次消解法), 消化大米标准物质(GBW 10010), 采用ICP-MS法测定铝, 同时添加回收率来验证不同处理方法的准确性与可靠性。结果 对测定结果进行比较分析, 前3种消解法的测定值均低于标准值; 最后一种消解法在标准值允许范围内; 4种前处理方法的检出限在0.42~0.52 mg/kg之间, 相对标准偏差3.61%~4.77%(n=6), 加标回收率在92.2%~97.8%之间。结论 谷物样品中可能存在酸不溶铝, 采取硝酸-氢氟酸-双氧水体系微波消解, 加高氯酸二次消解法的方式能将其消解完全, 该法可用于谷物样品中铝的测定。

英文摘要:

      Objective To establish an accurate method for the determination of the aluminum in the grain samples by inductively coupled plasma mass spectrometry (ICP-MS). Methods Four kinds of different pre-treatment methods were studied, including dry ashing, microwave digestion (HNO3-H2O2 digestive system), microwave digestion (HNO3-HF-H2O2 digestive system) and microwave digestion (HNO3-HF-H2O2 digestive system, then melted by adding perchloric acid). National standard substance rice power (GBW 100l0) was digested and its aluminum content was determined by ICP-MS. Accuracy and reliability of these methods were verified by recovery test. Results The analysis of the determination showed that the results of these previous 3 kinds of pre-treatment methods were lower than the standard value and the last one was within the standard value. The detection limits of these four kinds of pre-treatment methods varied from 0.42 to 0.52 mg/kg, relative standard deviations (RSDs) varied from 3.61% to 4.77% (n=6) and recoveries were between 92.2% and 97.8%. Conclusion Acid insoluble aluminum exists in the grain samples. Microwave digestion(HNO3-HF-H2O2 digestive system, then melted by adding perchloric acid) can be used in the detection of grain samples as the acid insoluble aluminum can be released through this pre-treatment method.