混酸密闭分解电感耦合等离子质谱法快速测定磷矿中的碘

孙霞; 郑松; 岳晓岚; 贾双琳; 杨刚; 赵平

孙霞,郑松,岳晓岚,贾双琳,杨刚,赵平.混酸密闭分解电感耦合等离子质谱法快速测定磷矿中的碘[J].贵州地质,2017,34(1):55-59，54

混酸密闭分解电感耦合等离子质谱法快速测定磷矿中的碘

Rapid Determination of Iodine in Phosphate Ores by Mixed Acid Decomposition under Closed Vessel Condition and Inductively Coupled Plasma-Mass Spectrometry

DOI：

中文关键词: ICP-MS 磷矿碘稀氨水

英文关键词:ICP-MS Phosphate ores Iodine Dilute ammonia solution

基金项目:贵州省地质矿产勘查开发局地质科研项目[合同编号：黔地矿科合（2015）23号]

作者	单位
孙霞	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550018；
郑松	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550019；
岳晓岚	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550020；
贾双琳	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550021；
杨刚	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550022；
赵平	1.贵州省地质矿产中心实验室，贵州贵 550018；2.国土资源部贵阳矿产资源监督检测中心，贵州贵阳550018；3.中国地质大学（武汉）材料与化学学院，湖北武汉430074

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中文摘要:

磷矿中碘元素的快速测试方法：以磷酸和高氯酸混合酸密闭加热分解磷矿，用盐酸羟胺使碘还原成低价态，加氨水调节溶液至碱性。取上清液5mL，用稀氨水1∶1稀释后，用电感耦合等离子质谱仪测试磷矿中碘的含量。结果表明，加氨水浓度30%时，测试的结果最理想，取上清液用2%氨水稀释，可以解决不同磷矿的仪器测试带来的仪器堵塞和熄火的问题。两种磷矿国家一级标准物质GBW07210和GBW07211电感耦合等离子质谱仪测试结果均与推荐值吻合。测定误差均在允许范围内，方法的检出限为0.25 μg/g，加标回收率为99.6%~103.5%。精密度为2.32%~3.21%，结果良好。实验结果表明该方法具有良好的稳定性和可靠性。

英文摘要:

Rapid testing method of iodine in phosphate Ores：sample was decomposed by mixed acid of phosphoric acid and perchloric acid under closed vessel condition and iodine in the solution was reduced to low valance by hydroxylamine hydrochloride，sample solution was adjusted to weak alkaline using ammonia solution5 mL supernatant was taken to be diluted by dilute ammonia solution before tested by inductively coupled plasma mass spectrometryThe results showed that，the best results were obtained When 30% ammonia was added and the problems of instrument clogging and flameout were solved when solution was diluted by 2% ammonia solution before tested by inductively coupled plasma mass spectrometry.The method has been applied to the determination of iodine in National Standard Materials GBW07210 and GBW07211 and the test results were consistent with the recommended values.Measurement error were within the allowable range.The detection limit of the method for iodine was 0.25 μg/g and the recoveries were 99.6% ～103.5%The precisions were 2.32%～3.21%.Phosphorite combination samples from Weng’an County，Guizhou Province which have different iodine content were analyzed by two laboratories and the measurement error between the two laboratories were within the allowable rangeThe experimental results showed that the method had good stability and reliability.

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