Determination of Major Elements in Sepoilite by Inductively Coupled Plasma-Optical Emission Spectrometry with Opening Acid Dissolution
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摘要: 海泡石是一种应用广泛的纤维状富镁硅酸盐黏土矿物，主要成分为硅和镁，伴有铝钾钠等杂质，测定海泡石主量成分含量对于矿物性能的综合评价具有重要意义。海泡石主量元素分析通常采用经典化学法，样品碱熔处理后使用容量法、光度法、原子吸收光谱法测定，操作繁琐，耗时长，且无法同时测定钾钠。本文建立了一种氢氟酸-硝酸-高氯酸敞口酸溶样品，ICP-OES测定海泡石中氧化铝等主量成分的方法。对氢氟酸的用量进行了优化，选择Al 396.153nm、Ti 334.940nm、K 766.490nm、Na 589.592nm、Ca 422.673nm、Mg 285.213nm、Fe 238.204nm作为分析谱线，采用轴向观测方式进行测量。由于海泡石中的镁含量较高，用ICP-OES测定时存在基体效应，通过配制系列高镁混合标准溶液以匹配基体。ICP-OES法同时测定铝钛钾钠钙镁铁各元素标准曲线线性相关系数均大于0.9990，方法检出限为0.53~3.25μg/g，测定结果的相对标准偏差（RSD，n=10）为0.66%~5.65%，各元素回收率为95.3%~108.5%。本方法采用的酸溶前处理方式较碱熔操作更加简单，测定结果与经典化学方法所得结果吻合较好，能够满足海泡石样品的分析需求。
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关键词:
- 海泡石 /
- 氢氟酸-硝酸-高氯酸敞口酸溶 /
- 铝 /
- 主量元素 /
- 电感耦合等离子体发射光谱法
Abstract:BACKGROUNDSepiolite is a widely used fibrous magnesium-rich silicate clay mineral. Sepiolite is mainly composed of silicon and magnesium, with minor aluminum, potassium, sodium and other impurities. Determination of the major element of sepiolite usually adopts the classical chemical analytical method. After the alkali melting treatment, the sample is determined by volumetric method, photometry and atomic absorption spectrometry, which is inefficient and time-consuming. Moreover, potassium and sodium cannot be simultaneously determined. OBJECTIVESTo find an efficient method for the determination of seven major elements in sepiolite. METHODSThe samples were digested by hydrofluoric acid, nitric acid, and perchloric acid. Contents of major elements such as Al2O3 were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The dosage of hydrofluoric acid was optimized. The analytical spectral lines were Al 396.153nm, Ti 334.940nm, K 766.490nm, Na 589.592nm, Ca 422.673nm, Mg 285.213nm and Fe 238.204nm, and elements were determined by axial observation. The content of magnesium in sepiolite was high, and there was a certain matrix effect during ICP-OES analysis. A series of high magnesium mixed standard solutions were prepared to match the matrix. RESULTSThe linear correlation coefficient of the standard curve of each element was greater than 0.9990, the detection limits of the method were 0.53-3.25μg/g, the relative standard deviations (RSD, n=10) of the measured results were 0.66%-5.65%, and the recoveries of each element were 95.3%-108.5%. CONCLUSIONSAcid dissolution is easy to operate compared with the alkali fusion method. The results are consistent with those obtained by classical chemical analytical methods and thus meet the analytical requirements of sepiolite samples. -
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表 1 系列混合标准溶液中元素的浓度
Table 1. Concentrations of elements in mixed standard solution series
标准溶液编号 各元素浓度(μg/mL) Al2O3 TiO2 K2O Na2O CaO MgO Fe2O3 标准1 10 0.5 1 0.5 5 20 5 标准2 20 1 2 1 10 40 10 标准3 50 2.5 5 2.5 20 100 20 标准4 100 5 10 5 50 200 50 标准5 200 10 20 10 100 400 100 
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表 2 不同氢氟酸用量下各组分的测定结果(氧化物)
Table 2. Analytical results of components under different HF dosages
组分 不同氢氟酸用量各组分的测定值(%) 2.0mL 3.0mL 4.0mL 5.0mL 6.0mL 7.0mL Al2O3 3.76 4.15 4.55 4.57 4.58 4.54 TiO2 0.13 0.16 0.18 0.18 0.18 0.18 K2O 0.19 0.22 0.27 0.27 0.28 0.27 Na2O 0.06 0.09 0.10 0.11 0.10 0.11 CaO 2.05 2.29 2.50 2.51 2.48 2.53 MgO 14.73 17.56 18.09 18.06 18.04 18.08 Fe2O3 1.18 1.35 1.48 1.45 1.43 1.47
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表 3 方法检出限和准确度
Table 3. Detection limit and accuracy tests of the method
组分 样品含量(%) 加标量(%) 测得总量(%) 回收率(%) 检出限(μg/g) Al2O3 4.57 5 9.45 98.8 0.53 TiO2 0.18 0.2 0.39 103.4 1.43 K2O 0.27 0.2 0.45 95.3 3.25 Na2O 0.11 0.1 0.23 108.5 1.18 CaO 2.51 2.5 4.89 97.5 1.69 MgO 18.06 10 28.45 101.4 2.46 Fe2O3 1.45 1.5 3.02 102.3 1.36
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表 4 方法精密度
Table 4. Precision tests of the method
组分 分次测定值(%) 平均值(%) RSD(%) Al2O3 4.62 4.52 4.59 4.60 4.57 4.57 0.94 4.60 4.56 4.59 4.52 4.49 TiO2 0.17 0.18 0.18 0.18 0.18 0.18 2.73 0.17 0.18 0.18 0.18 0.17 K2O 0.27 0.27 0.27 0.27 0.28 0.27 1.55 0.28 0.27 0.27 0.27 0.27 Na2O 0.10 0.11 0.11 0.12 0.11 0.11 5.65 0.11 0.12 0.11 0.11 0.12 CaO 2.51 2.56 2.45 2.47 2.49 2.51 2.88 2.65 2.42 2.61 2.51 2.47 MgO 17.98 18.21 18.05 17.96 17.93 18.06 0.66 18.13 17.85 18.13 18.19 18.14 Fe2O3 1.45 1.46 1.45 1.45 1.42 1.45 1.65 1.43 1.46 1.45 1.44 1.51
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表 5 分析结果对比
Table 5. Comparison of different methods
组分 对比方法 测定值(%) 本文方法测定值(%) Al2O3 容量法 4.65 4.57 TiO2 分光光度法 0.18 0.18 K2O 原子吸收光度法 0.27 0.27 Na2O 原子吸收光度法 0.12 0.11 CaO 容量法 2.49 2.51 MgO 容量法 18.15 18.06 Fe2O3 分光光度法 1.48 1.45
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