【引用本文】 何海洋, 董学林, 储溱, 等. 封闭酸溶-硅钼蓝比色分光光度法测定地质样品中的硅[J]. 岩矿测试, 2019, 38(5): 576-583. doi: 10.15898/j.cnki.11-2131/td.201708230132
HE Hai-yang , DONG Xue-lin , CHU Qin , et al. Determination of Silica in Geological Samples by Silicon-Molybdenum Blue Spectrophotometry Using High-pressure Acid Digestion[J]. Rock and Mineral Analysis, 2019, 38(5): 576-583. doi: 10.15898/j.cnki.11-2131/td.201708230132

封闭酸溶-硅钼蓝比色分光光度法测定地质样品中的硅

1. 湖北省地质实验测试中心, 湖北 武汉 430034;

2. 国土资源部稀土稀有稀散矿产重点实验室, 湖北 武汉 430034;

3. 华中科技大学化学与化工学院, 湖北 武汉 430074

收稿日期: 2018-06-23  修回日期: 2018-09-28 

基金项目: 国家重点研发计划项目“重点领域急需化学成分量标准物质研究”(2016YFF0201103);国土资源公益性行业科研专项“典型金属矿选冶样品及小取样量分析方法研究”(201211056)

作者简介: 何海洋,工程师,主要从事岩矿测试及研究工作。。

Determination of Silica in Geological Samples by Silicon-Molybdenum Blue Spectrophotometry Using High-pressure Acid Digestion

1. Hubei Province Geological Experimental Testing Center, Wuhan 430034, China;

2. Key Laboratory of Rare Mineral, Ministry of Land and Resources, Wuhan 430034, China;

3. School of Chemistry Engineering, Huazhong University of Science & Technology, Wuhan 430074, China

Received Date: 2018-06-23
Revised Date: 2018-09-28

摘要:由于聚合态的硅酸无法与钼酸根定量络合,采用硅钼蓝比色分光光度法测定地质样品中的硅,其关键在于如何将固体试样消解制备成溶液且保证硅酸全部以单分子状态存在。本文以氢氟酸-硝酸封闭酸溶消解地质样品,使样品中的硅完全转化为氟硅酸稳定存在于溶液中;再加入硼酸和钼酸铵,使过量的氢氟酸与硼酸生成稳定的BF4-配离子,此步骤代替了蒸干赶除氢氟酸,从而避免了赶酸过程中硅与氟离子转化为气态SiF4而挥发损失,在钼酸铵作用下,硅则充分转变为硅钼杂多酸。在显色过程中通过加入丙酮显著提高了硅钼黄的稳定性,且在一定程度上增加了吸光度,从而改善了硅钼蓝分光光度法测定硅的显色效果。该方法避免了常规碱熔消解样品后在酸化过程中硅酸易聚合、引入大量熔剂造成空白偏高等问题,经岩石、土壤、沉积物和石英岩国家标准物质分析验证,测试结果准确且重现性好(RSD<1%,n=10)。该方法适用于一般地质样品中二氧化硅的快速、准确分析。

关键词: 岩石, 土壤, 沉积物, , 氢氟酸-硝酸酸溶, 密闭消解, 分光光度法

Determination of Silica in Geological Samples by Silicon-Molybdenum Blue Spectrophotometry Using High-pressure Acid Digestion

KEY WORDS: rock, soil, sediment, silica, HF-HNO3 dissolution, high-pressure digestion, spectrophotometry

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封闭酸溶-硅钼蓝比色分光光度法测定地质样品中的硅

何海洋, 董学林, 储溱, 宋洲