采用HF-HNO_3-HClO_4混酸消化样品,HNO_3溶解盐类,火焰原子吸收光谱法直接测定试液中钙、铜、铁、锰的含量.对共存离子的干扰情况进行了考察,发现大量的Si对测定有干扰,在处理样品时通过生成SiF_4除去;磷、铝、钛等元素对钙的化学干扰,通过加入释放剂SrCl_2消除.背景吸收使用氘灯扣除.采用标准曲线法测定,Ca、Cu、Fe、Mn的校准曲线的线性范围分别为0.00～20.00μg/mL、0.00～6.00弘g/mL、0.00～10.00 μg/mL、0.00～6.00μg/mL,检出限分别为0.000 3μg/mL、0.001 3 μg/mL、0.002 6μg/mL、0.006 9 μg/mL.方法用于云冈石窟风化岩石中钙、铜、铁、锰的测定,相对标准偏差分别为2.8%、3.0%、1.4%、2.9%,加标回收率在96%～110%之间.
The sample was dissolved in mixed acid of HF-HNO_3-HClO_4 while the produced salts were dissolved in HNO_3. The content of calcium, copper, iron and manganese in sample solution was directly determined by flame atomic absorption spectrometry. The interference of coexisting ions was tested. It was found that a mass of silicon could interfere with the determination, but they could be eliminated in form of SiF_4 during sample preparation. The chemical interference from phosphorus, aluminium and titanium could be eliminated by adding SrCl_2. The background absorption was deducted using deuterium lamp. The determination was conducted with standard curve method. The linear range of calcium, copper, iron and manganese was 0-20. 00 μg/mL, 0. 00-6. 00μg/mL, 0. 00-10. 00 μg/mL and 0. 00-6.00 μg/mL, and the detection limit was 0. 000 3 μg/mL, 0. 001 3μg/mL, 0. 002 6 μg/mL and 0. 006 9 μg/mL, respectively. This method was applied to the determination of calcium, copper, iron and manganese in weathering rock of Yungang Grottoes, with the relative standard deviations (RSD) of 2.8%, 3.0%, 1.4% and 2.9%, and the recoveries in the range of 90%-110%.
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