Determination of Trace Selenium in High-Carbon and High-Sulfur Geological Samples by Thiol Cotton Fiber Separation-Atomic Fluorescence Spectrometry
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摘要:
氢化物发生-原子荧光光谱法（HG-AFS）应用于测定地质样品中的痕量硒具有较高的灵敏度，但复杂的基质仍会增加分析难度，尤其是富含有机质样品与硫化物样品中的有机碳、复杂配合物和共存离子等带来的干扰，故样品前处理十分重要。采用常规的巯基棉（thiol cotton fibre，TCF）富集分离方法处理富含有机质样品与硫化物样品时，常会出现回收率不稳定、TCF过早饱和的现象。因此，本文针对富含有机质样品，使用双TCF柱法，通过两次吸附可以有效减少有机质的干扰；针对硫化物样品，可通过增加TCF的用量或者减少称样量来提高硒的回收率。标准物质和实际样品的测定结果表明优化的方法可满足分析要求，对富有机质样品，硒的回收率大于95.1%±0.37%；对硫化物样品，硒的回收率大于95.5%±1.92%。同时，研究也表明，采用微波消解处理样品，能够有效地避免硒在消解过程中的损失。改进后的方法提升了富集分离效果，适用于有机质和硫化物地质样品中的痕量硒（ng/g~μg/g级）分析要求。
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关键词:
- 高碳高硫地质样品 /
- 硒 /
- 微波消解 /
- 巯基棉 /
- 氢化物发生-原子荧光光谱法
Abstract:BACKGROUND Hydride generation-atomic fluorescence spectroscopy (HG-AFS) is highly sensitive for the determination of trace selenium in geological samples. However, the complex matrix increases the analysis difficulty, especially owing to interference caused by organic carbon, complicated complexes, and coexisting ions in samples rich in organic matter and sulfides. Therefore, sample pretreatment is important. The use of conventional thiol cotton fiber (TCF) to enrich and separate selenium often leads to unstable recovery and premature saturation of the TCF when dealing with samples rich in organic matter and sulfides.
OBJECTIVES To establish a method suitable for the determination of trace selenium in geological samples rich in organic matter and sulfides.
METHODS For samples rich in organic matter, a double TCF column (mTCF=0.15g) was used to carry out adsorption twice. The recovery for high-sulfur geological samples could be increased either by increasing the amount of TCF (mTCF ≤ 0.2g) or reducing the sample amount.
RESULTS The measurement results for the reference materials and actual samples showed that the optimized method satisfied the analysis requirements as selenium recoveries of >95.1% and >95.5% were achieved for the organic-rich and sulfide samples, respectively. Microwave digestion can effectively avoid the loss of selenium during digestion; the measured selenium content was consistent with that reported in the literature.
CONCLUSIONS The improved method is suitable for geological samples rich in organic matter and sulfides, which can be used to determine trace selenium (ng/g to μg/g levels) in geological samples.
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表 1 优化后的实验条件和流程
Table 1. Optimized experimental conditions and processes in this study
样品处理和分析步骤 具体操作流程和实验条件 样品消解 浓硝酸(6mL)，氢氟酸(2mL)，200℃微波消解90min 硒的还原 ①样品蒸干后赶酸，加入15mL 5mol/L盐酸定容，静置过夜
②沸水浴30min，冷却至室温TCF富集分离硒 ①5mol/L的盐酸介质，15mL样品+15mL超纯水，调节至2.5mol/L的盐酸介质
②TCF柱准备：0.15~0.2g，放入微柱中压实
③洗涤：2.5mL+2.5mL超纯水洗涤TCF柱
④平衡：2.5mL+2.5mL 2.5mol/L盐酸平衡TCF柱
吸附Se(Ⅳ)：30mL样品以0.05mL/s通过TCF柱硒的解吸 ①取下TCF后转移比色管中，加入2mL 12mol/L浓盐酸、2滴浓硝酸
②沸水浴，3min，冷却至室温
③离心：将絮状溶液离心后，转移上层清液
④多次回收TCF上的硒：3mL+5mL超纯水，清洗比色管，充分振荡
⑤多次离心，将上层清液混合，稀释至上机浓度准备测试HG-AFS测试 载流：5%盐酸溶液还原剂：2%硼氢化钾溶液 
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表 2 不同处理体系测定富有机质地质样品中的硒含量结果
Table 2. Analytical results of selenium content in organic-rich geological samples pretreated by different processing systems
处理体系分组 样品编号 岩性 硒推荐值(μg/g) 硒测定值(n=2)(μg/g) 硒回收率(%) 硒平均回收率(%) T-1 SGR-1b 油气页岩 3.5 2.87±0.01 82.0 77.6±4.43 SGR-1b 油气页岩 3.5 2.56±0.04 73.1 GBW07303 水系沉积物 1±0.2 0.87±0.05 87.0 85.5±1.50 GBW07303 水系沉积物 1±0.2 0.84±0.06 84.0 GBW07407 土壤 1.34±0.17 1.07±0.07 79.9 80.6±0.75 GBW07407 土壤 1.34±0.17 1.09±0.01 81.3 MA-4 黑色页岩 7.1 5.56±0.08 78.3 76.5±1.83 MA-4 黑色页岩 7.1 5.30±0.11 74.6 MA-5 黑色页岩 33.2 27.14±0.16 81.7 83.1±1.37 MA-5 黑色页岩 33.2 28.05±0.14 84.5 T-2 SGR-1b 油气页岩 3.5 3.47±0.14 99.1 101.1±2.00 SGR-1b 油气页岩 3.5 3.61±0.05 103.1 GBW07303 水系沉积物 1±0.2 0.90±0.03 90.0 91.5±1.50 GBW07303 水系沉积物 1±0.2 0.93±0.02 93.0 GBW07407 土壤 1.34±0.17 1.37±0.09 102.2 100.0±2.24 GBW07407 土壤 1.34±0.17 1.31±0.04 97.8 MA-4 黑色页岩 7.1 6.73±0.19 94.8 96.4±1.62 MA-4 黑色页岩 7.1 6.96±0.07 98.0 MA-5 黑色页岩 33.2 34.1±0.15 102.7 99.4±3.31 MA-5 黑色页岩 33.2 31.9±0.11 96.1 T-3 SGR-1b 油气页岩 3.5 3.44±0.06 98.3 103.6±5.29 SGR-1b 油气页岩 3.5 3.81±0.01 108.9 GBW07303 水系沉积物 1±0.2 1.02±0.01 102.0 101.5±0.50 GBW07303 水系沉积物 1±0.2 1.01±0.05 101.0 GBW07407 土壤 1.34±0.17 1.28±0.02 95.5 95.1±0.37 GBW07407 土壤 1.34±0.17 1.27±0.03 94.8 MA-4 黑色页岩 7.1 6.82±0.12 96.1 99.2±3.10 MA-4 黑色页岩 7.1 7.26±0.09 102.3 MA-5 黑色页岩 33.2 35.67±0.24 107.4 106.2±1.23 MA-5 黑色页岩 33.2 34.85±0.17 105.0 注：n为测定次数，"硒测定值(n=2)"为两次测定平均值。T-1组为单柱法不加H2O2体系；T-2为单柱法加H2O2体系；T-3为双柱法不加H2O2体系。
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表 3 不同处理体系测定硫化物样品中硒含量结果
Table 3. Analytical results of selenium content in sulfide samples pretreated by different processing systems
处理体系分组 样品编号 样品性质 TCF用量(g) 硒推荐值(μg/g) 硒测定值(n=2)(μg/g) 硒回收率(%) 硒平均回收率(%) S-1 GBW07237 锌矿石 0.15 2.3±0.6 2.05±0.04 89.1 89.6±0.43 GBW07237 锌矿石 2.3±0.6 2.07±0.04 90.0 GBW07270 闪锌矿 0.15 3 2.73±0.03 91.0 89.2±1.83 GBW07270 闪锌矿 3 2.62±0.03 87.3 MA-1 全岩硫化物 0.15 39.3 29.23±0.05 74.4 73.9±0. 47 MA-1 全岩硫化物 39.3 28.86±0.04 73.4 MA-2 全岩硫化物 0.15 27.6 23.94±0.07 86.7 86.2±0.58 MA-2 全岩硫化物 27.6 23.62±0.07 85.6 MA-3 辉钼矿 0.15 0.78 0.65±0.01 83.3 80.8±2.56 MA-3 辉钼矿 0.78 0.61±0.02 78.2 S-2 GBW07237 锌矿石 0.20 2.3±0.6 2.37±0.05 103.0 103.3±0.22 GBW07237 锌矿石 2.3±0.6 2.38±0.01 103.5 GBW07270 闪锌矿 0.20 3 3.11±0.01 103.7 99.2±4.50 GBW07270 闪锌矿 3 2.84±0.03 94.7 MA-1 全岩硫化物 0.20 39.3 38.35±0.02 97.6 97.4±0.18 MA-1 全岩硫化物 39.3 38.21±0.04 97.2 MA-2 全岩硫化物 0.20 27.6 28.89±0.09 104.7 103.4±1.23 MA-2 全岩硫化物 27.6 28.21±0.08 102.2 MA-3 辉钼矿 0.20 0.78 0.73±0.01 93.6 95.5±1.92 MA-3 辉钼矿 0.78 0.76±0.03 97.4 注：n为测定次数，"硒测定值(n=2)"为两次测定平均值。
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表 4 不同处理步骤硒标准溶液的回收率
Table 4. Recovery of selenium standard solution treated by different processing steps
分组 编号 硒含量(ng) 消解前添加无硒玄武岩 消解后添加无硒玄武岩 还原处理 TCF纯化后硒含量(ng) 硒回收率(%) 硒平均回收率(%) B-1 β-1 0 √ × √ 0 - - β-2 0 √ × √ 0 - B-2 β-3 150 × × × 107.01 71.3 72.3±0.92 β-4 150 × × × 109.77 73.2 B-3 β-5 150 × × √ 112.89 75.3 78.3±3.08 β-6 150 × × √ 122.12 81.4 B-4 β-7 150 √ × √ 151.97 101.3 100.5±0.80 β-8 150 √ × √ 149.57 99.7 B-5 β-9 150 × √ √ 153.56 102.4 101.9±0.44 β-10 150 × √ √ 152.24 101.5
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表 5 改进后的方法与不同研究中硒的测定值比较
Table 5. Comparison of the measured values of selenium with improved method (this work) and other studies
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