PDF (1503K)
摘要
通过改变混合酸(盐酸-硝酸-氢氟酸-高氯酸)中高氯酸的比例,采用石墨管加热消解和电热板加热消解2种方式,残渣用逆王水提取,3%稀硝酸定容测定,建立了一种理想的酸分解方法用于电感耦合等离子体质谱/发射光谱法(ICP-MS/OES)测定地球化学样品主、次、痕量元素。结果表明,当使用10 mL逆王水、5 mL氢氟酸、石墨管加热消解(加入2~3 mL高氯酸),或电热板加热消解(加入3~4 mL高氯酸分解试样),使用10 mL 50%逆王水提取,对主、次、痕量元素分解效果都有提高,尤其对主量元素分解效果的提高最为明显。测定结果显示,5种元素方法检出限在0.011~42.8 μg/g,相对标准偏差(n=9)在2.06%~7.56%,精密度和准确度均满足地质实验室质量管理规范要求,可快速、准确测定地球化学样品中的多元素。
Abstract
An ideal sample acid decomposition method is established and used to determine major,minor and trace elements in geochemical samples by inductively coupled plasma mass spectrometry/emission spectroscopy (ICP-MS/OES) through changing the ratio of perchloric acid in the mixed acid (hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid),employing graphite tube heating digestion and hot plate heating digestion modes,extracting the residue by reverse aqua regia,and using 3% dilute nitric acid for constant volume and measurement.Results show that the decomposition efficiencies of major,minor and trace elements can be improved by using 10 mL reverse aqua regia,5 mL hydrofluoric acid,graphite tube heating digestion with 2-3 mL of perchloric acid,or by using a hot plate for digestion,adding 3-4 mL of perchloric acid to decompose the sample and using 10 mL of 50% reverse aqua regia to extract.Especially the decomposition effect of major elements is improved more significantly.Detection results show that detection limit for five elements is between 0.011-42.8 μg·g-1,and relative standard deviation (n=9) is between 2.06% and 7.56%.Both the precision and accuracy of this method meet the requirement from geological laboratory management regulations.Multiple elements in geochemical samples can be determined quickly and accurately by this method.
关键词
地球化学样品
/
电感耦合等离子体质谱/发射光谱法
/
电热板加热消解
/
石墨管加热消解
Key words
geochemical samples
/
ICP-MS/OES
/
hot plate heating digestion
/
graphite tube heating digestion
电感耦合等离子体质谱/发射光谱法测定地球化学样品前处理条件的优化选择[J].
现代化工, 2021, 41(7): 245-250 DOI:10.16606/j.cnki.issn0253-4320.2021.07.050