摘要
研究了盐酸-硝酸-氢氟酸-高氯酸酸溶和氢氧化钠碱熔两种测定铝土矿石样品中镓的前处理方法,利用电感耦合等离子体发射光谱法(ICP-AES)进行测定。对熔矿试剂及条件、分析谱线的选择和元素的干扰进行了讨论,采用不同含量的铝土矿石国家标准物质样品进行了条件实验。分析结果表明:采用盐酸-硝酸-氢氟酸-高氯酸溶解样品,会导致铝土矿石样品溶解不完全,得到的数据失真;而采用氢氧化钠碱熔法处理铝土矿石样品后,用ICP-AES法测定,镓的测定值准确度高,方法检出限为0.15μg/g,相对标准偏差(RSD,n=11)为2.51%～5.97%,回收率为94.8%～108.2%。该方法灵敏度高,精密度好,分析时间短,易于流程操作。方法经国家一级标准物质分析验证,测定结果与标准值相符,特别适用于铝土矿石样品中镓的测定。
Two different sample pretreatment methods-NaOH alkali fusion method and HCl-HNO3-HF-HClO4 acid dissolution method were compared in order to quantify Ga in bauxite ore samples by inductively coupled plasma-atomic emission spectrometry（ICP-AES）.The loaded reagents,chemical procedure,selection of analysis spectral lines and interferences are discussed in this paper.National Standard Reference bauxite ore samples with different Ga contents were analyzed by using both sample pretreatment methods.The analytical results indicate that the bauxite ore samples were incompletely dissolved by using HCl-HNO3-HF-HClO4 acids,which provided an incorrect result.Meanwhile,the pretreatment for bauxite ore samples with sodium hydroxide by alkali fusion provided higher accuracy and precision,giving a range of 2.51%-5.97%（RSD,n=11） and a detection limit for Ga of 0.15 μg/g with recoveries of the method ranging from 94.8% to 108.2%.The reliability of the alkali fusion method has been tested by quantification of Ga in National Standard Reference materials and the results were in agreement with the certified values.This method has advantages of rapid analysis,simple operation and more efficient measurement of Ga in bauxite ore samples.
出处
《岩矿测试》
CAS
CSCD
北大核心
2011年第4期481-485,共5页
Rock and Mineral Analysis
基金
贵州省地质勘查基金(周转金)矿产项目(TK2009-006)
关键词
镓
铝土矿
电感耦合等离子体发射光谱法
酸溶
氢氧化钠碱熔
gallium
bauxite ore
inductively coupled plasma-atomic emission spectrometry
acid dissolution
sodium hydroxide alkali fusion
