Determination of 8 Metal Elements in Soil by High-resolution Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion
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摘要:
微波消解结合电感耦合等离子体质谱(ICP-MS)是土壤样品中金属元素测定的常用方法，其前处理可以采用不同的消解体系，但是消解体系对分析结果的准确性影响较大。此外，应用ICP-MS测定某些元素时干扰的存在会影响结果的准确性。基于上述问题，本文优选三个酸体系微波消解溶样，采用高分辨电感耦合等离子体质谱(HR-ICP-MS)测定土壤样品中8种金属元素(Cr、Co、Ni、Cu、Zn、Pb、Cd和U)的含量，对比研究了由不同用量硝酸、盐酸、氢氟酸混合组成的三个酸消解体系对国家土壤标准物质的消解效果，确定了最优前处理方法。结果表明：经国家土壤标准物质验证，采用HR-ICP-MS检测，在不需要干扰校正的情况下，酸体系Ⅰ(6mL硝酸+3mL盐酸+3mL氢氟酸)和酸体系Ⅱ(2mL硝酸+6mL盐酸+1mL氢氟酸)的测定值与标准值相吻合，方法检出限为0.001~0.715μg/g，精密度(RSD，n=6)小于7.0%。从消解情况、准确度和精密度比较，酸体系Ⅰ稍优于酸体系Ⅱ；从酸用量比较，酸体系Ⅱ酸用量最少。两种酸体系的样品处理方法均具有较高的适用性和可靠性，都可用于土壤样品中8种金属元素含量的直接测定。
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关键词:
- 土壤 /
- 金属元素 /
- 微波消解 /
- 酸消解 /
- 高分辨电感耦合等离子体质谱法
Abstract:BACKGROUND Microwave digestion combined with inductively coupled plasma-mass spectrometry (ICP-MS) is a commonly used method for the determination of metal elements in soil samples. Different solvents can be used in the pretreatment, and the digestion method has a great influence on the accuracy of the analysis results. In addition, the accuracy of the results will be affected by the interference in the determination of some elements by ICP-MS.
OBJECTIVES To accurately determine metal elements in soil samples by high resolution-inductively coupled plasma-mass spectrometry (HR-ICP-MS).
METHODS Soil samples were digested by microwave using three different solvents, and 8 metal elements (Cr, Co, Ni, Cu, Zn, Pb, Cd and U) were determined by HR-ICP-MS. The digestion effects of the three acid digestion methods using different amounts of nitric acid, hydrochloric acid and hydrofluoric acid on certified soil reference materials were studied, and the optimal pretreatment procedure was determined.
RESULTS The proposed procedures have been verified by national soil reference materials. It was found that the measured values of digestion method Ⅰ(6mL HNO3+3mL HCl+3mL HF) and digestion method Ⅱ(2mL HNO3+6mL HCl+1mL HF) were consistent with the certified values, using HR-ICP-MS without interference correction. The detection limits of both procedures were 0.001-0.715μg/g. The relative standard deviations (RSD, n=6) were all less than 7.0%. In terms of digestion, accuracy and precision, acid system Ⅰ was slightly better than acid system Ⅱ, but acid system Ⅱ had the least amount of acid.
CONCLUSIONS The two preferred procedures have high applicability and reliability, and can be used for the direct determination of 8 metal elements in soil samples.
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表 1 微波消解实验条件
Table 1. Experimental conditions for microwave digestion
消解步骤 升温时间(min) 目标温度(℃) 保温时间(min) 1 5 120 10 2 10 160 20 3 10 185 50 
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表 2 标准物质中金属元素的分析结果
Table 2. Analytical results of metal elements in certified reference materials
金属元素 标准物质编号 标准值(μg/g) 酸体系Ⅰ 酸体系Ⅱ 酸体系Ⅲ 测定值(μg/g) 相对误差(%) ΔlgC 测定值(μg/g) 相对误差(%) ΔlgC 测定值(μg/g) 相对误差(%) ΔlgC Cr GBW07385 80±5 83.3 4.1 0.02 77.5 -3.1 0.01 78.2 -2.3 0.01 GBW07407 410±23 399 -2.7 0.01 431 5.1 0.02 414 1.0 0 Co GBW07385 16.0±0.6 15.8 -1.3 0.01 16.0 0 0 14.9 -6.9 0.03 GBW07407 97±6 102 5.2 0.02 94.6 -2.5 0.01 103 6.2 0.03 Ni GBW07385 38±2 40.1 5.5 0.02 41.4 8.9 0.04 38.8 2.1 0.01 GBW07407 276±15 296 7.2 0.03 281 1.8 0.01 293 6.2 0.03 Cu GBW07385 35±2 36.4 4.0 0.02 37.5 7.1 0.03 33.7 -3.7 0.02 GBW07407 97±6 104 7.2 0.03 107 10.0 0.04 103 6.2 0.03 Zn GBW07385 96±4 93.7 -2.4 0.01 95.7 -0.3 0 103 7.3 0.03 GBW07407 142±11 136 -4.2 0.02 142 0 0 156 9.9 0.04 Pb GBW07385 32±3 33.0 3.1 0.01 31.7 -0.9 0 28.1 -12.0 0.06 GBW07407 14±3 13.1 -6.4 0.03 13.0 -7.1 0.03 12.1 -14.0 0.06 Cd GBW07385 0.28±0.02 0.279 -0.4 0 0.279 -0.4 0 0.267 -4.6 0.02 GBW07407 0.08±0.02 0.076 -5.0 0.02 0.081 1.3 0.01 0.065 -19.0 0.09 U GBW07385 2.6±0.1 2.55 -1.9 0 2.70 3.8 0.02 2.55 -1.9 0.01 GBW07407 2.2±0.4 2.28 3.6 0.02 2.05 -6.8 0.02 2.08 -5.5 0.02
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表 3 三种消解体系的方法检出限和定量限
Table 3. Limits of detection and limits of quantification for the three acid digestion procedures
金属元素 酸体系Ⅰ 酸体系Ⅱ 酸体系Ⅲ 检出限(μg/g) 定量限(μg/g) 检出限(μg/g) 定量限(μg/g) 检出限(μg/g) 定量限(μg/g) Cr 0.715 2.38 0.309 1.03 0.887 2.96 Co 0.002 0.007 0.004 0.012 0.005 0.016 Ni 0.185 0.615 0.032 0.106 0.160 0.534 Cu 0.019 0.063 0.044 0.147 0.039 0.129 Zn 0.125 0.418 0.434 1.45 1.49 4.97 Pb 0.007 0.023 0.018 0.060 0.056 0.185 Cd 0.010 0.033 0.009 0.030 0.024 0.081 U 0.009 0.03 0.001 0.002 0.003 0.011
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表 4 三种酸消解体系比较
Table 4. Comparison of the three acid digestion procedures
比较项目 酸体系Ⅰ 酸体系Ⅱ 酸体系Ⅲ 称样量 0.25g 0.20g 0.10g 采用试剂 6mL硝酸+ 3mL盐酸+ 3mL氢氟酸 2mL硝酸+ 6mL盐酸+ 1mL氢氟酸 5mL硝酸+2mL盐酸+ 2mL氢氟酸，8~9mL硝酸、氢氟酸，5~10mL 50%硫酸 酸用量 12mL 9mL ＞20mL 消耗时间 3~4h 3~4h ＞15h 消解情况 余极少量残渣 余少量残渣 完全消解
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表 5 两种消解体系的方法准确度
Table 5. Accuracy tests of the two acid digestion procedures
标准物质编号 金属元素 标准值(μg/g) 酸体系Ⅰ 酸体系Ⅱ 测定值(μg/g) 相对误差(%) ΔlgC 测定值(μg/g) 相对误差(%) ΔlgC GBW07541 Cr 47±2 44.6 -5.1 0.02 51.2 8.9 0.04 Co 8.9±0.3 8.74 -1.8 0.01 9.54 7.2 0.03 Ni 22.2±0.7 22.8 2.7 0.01 24.2 9.0 0.04 Cu 16.9±0.6 16.6 -1.8 0.01 17.2 1.8 0.01 Zn 53±3 50.1 -5.5 0.02 56.0 5.7 0.02 Pb 20.0±0.8 20.0 0 0 18.7 -6.5 0.03 Cd 0.108±0.005 0.099 -8.3 0.04 0.114 5.6 0.02 U 12.5±0.5 12.3 -1.6 0.01 12.0 -4.0 0.02 GBW07564 Cr 166±4 151 -9.0 0.04 164 -1.2 0.01 Co 30.3±1.3 30.9 2.0 0.01 27.5 -9.2 0.04 Ni 60±2 61.1 1.8 0.01 56.6 -5.7 0.03 Cu 76±2 81.3 7.0 0.03 72.7 -4.3 0.02 Zn 181±3 182 0.6 0 196 8.3 0.03 Pb 71±3 73.1 3.0 0.01 66.6 -6.2 0.03 Cd 0.69±0.05 0.683 -1.0 0 0.740 7.2 0.03 U 9.0±0.5 9.58 6.4 0.03 9.58 6.4 0.03 GBW07568 Cr 34±3 34.3 0.9 0 30.8 -9.4 0.04 Co 7.0±0.2 6.46 -7.7 0.03 7.13 3.7 0.01 Ni 10.7±0.6 10.3 -3.7 0.02 11.0 2.8 0.01 Cu 15.1±0.5 15.2 0.7 0 15.4 2.0 0.01 Zn 65±3 59.7 -8.2 0.04 63.3 -2.6 0.01 Pb 39.5±1.2 40.3 2.0 0.01 38.7 -2.0 0.01 Cd 0.098±0.005 0.107 9.2 0.04 0.104 6.1 0.03 U 5.3±0.3 4.93 -7.0 0.03 4.92 -7.2 0.03 GBW07573 Cr 31±3 31.9 2.9 0.01 29.6 -4.5 0.02 Co 1.79±0.09 1.69 -5.6 0.02 1.66 -7.3 0.03 Ni 14.9±0.9 15.8 6.0 0.03 15.4 3.4 0.01 Cu 9.5±0.8 9.06 -4.6 0.02 8.90 -6.3 0.03 Zn (19) 17.6 -7.2 0.03 18.2 -6.7 0.02 Pb 11.3±0.7 12.0 6.2 0.03 11.1 -1.8 0.01 Cd (0.03) 0.019 -35.0 0.19 0.021 -31.0 0.16 U 1.45±0.08 1.58 9.0 0.04 1.40 -3.4 0.02 GSB07-3272-2015 Cr 63.6±5.6 62.5 -1.7 0.01 67.2 5.7 0.02 Co 11.2±1.6 10.7 -4.5 0.02 12.2 8.9 0.04 Ni 29.7±3.4 28.5 -4.0 0.02 31.4 5.7 0.02 Cu 71.8±4.1 70.3 -2.1 0.01 78.3 9.1 0.04 Zn 523±40 510 -2.5 0.01 504 -3.6 0.02 Pb 971±99 1002 3.2 0.01 896 -7.7 0.03 Cd 3.09±0.48 2.84 -8.1 0.04 3.35 8.4 0.04 U - - - - - - - 注：带括号数值为参考值；“-”表示标准样品中没有给出该元素的标准值。
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表 6 两种消解体系的方法精密度(n=6)
Table 6. Precision tests of the two acid digestion procedures (n=6)
金属元素 GBW07567标准值(μg/g) 酸体系Ⅰ 酸体系Ⅱ 6次测定值(μg/g) 平均值(μg/g) RSD(%) 6次测定值(μg/g) 平均值(μg/g) RSD(%) Cr 118±3 111 109 111 109 111 109 110 1.2 113 118 119 121 119 117 118 2.2 Co 17.6±0.7 17.2 17.1 17.1 17.3 17.4 17.2 17.2 0.7 17.7 18.4 18.6 19.2 19.1 18.1 18.5 3.2 Ni 60±2 59.9 57.4 59.1 60.4 61.0 60.4 59.7 2.2 60.1 62.1 61.9 61.9 61.8 58.3 61.0 2.5 Cu 41±2 40.7 40.2 41.7 41.6 42.6 41.7 41.4 2.1 43.5 48.9 45.0 45.9 44.5 42.4 45.0 5.0 Zn 102±2 103 100 102 100 100 101 101 1.2 97.3 100 103 105 105 99.3 102 3.1 Pb 36.7±1.0 39.0 36.6 37.2 38.2 37.0 38.4 37.7 2.5 36.2 38.0 38.4 40.1 39.8 39.1 38.6 3.6 Cd 0.30±0.03 0.277 0.313 0.315 0.317 0.292 0.334 0.308 6.5 0.303 0.313 0.366 0.334 0.319 0.320 0.326 6.8 U 4.0±0.3 3.92 3.46 3.76 3.65 3.60 3.62 3.67 4.3 3.57 3.62 3.95 3.91 3.86 3.68 3.77 4.3
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表 7 实际土壤样品中金属元素的分析结果
Table 7. Analytical results of metal elements in soil samples
金属元素 样品编号 酸体系Ⅰ 酸体系Ⅱ 相对偏差(%) 平均值(μg/g) RSD (%) 平均值(μg/g) RSD (%) Cr 样品1 55.6 3.2 56.9 4.7 1.2 样品2 58.4 0.9 56.4 3.4 1.7 样品3 52.2 2.1 49.0 0.6 3.2 Co 样品1 11.5 2.6 13.2 3.0 6.9 样品2 14.2 2.1 13.1 3.1 4.0 样品3 10.2 1.0 10.8 0.9 2.9 Ni 样品1 29.6 2.0 27.9 2.9 3.0 样品2 32.3 8.4 27.9 3.6 7.3 样品3 25.8 1.2 23.7 2.1 4.2 Cu 样品1 26.1 1.5 29.7 2.0 6.5 样品2 30.8 1.0 29.9 2.3 1.5 样品3 25.5 0.8 27.6 3.6 4.0 Zn 样品1 77.9 5.0 79.1 4.0 0.8 样品2 87.3 0.9 91.2 2.4 2.2 样品3 94.5 3.1 99.6 1.3 2.6 Pb 样品1 33.9 2.1 32.1 1.9 2.7 样品2 49.5 3.8 44.7 6.7 5.1 样品3 41.2 2.7 37.5 1.9 4.7 Cd 样品1 0.120 8.3 0.119 8.8 0.4 样品2 0.186 5.4 0.179 5.6 1.9 样品3 0.226 4.4 0.225 8.9 0.2 U 样品1 2.07 2.4 2.11 1.9 1.0 样品2 2.38 0.8 2.20 0.9 3.9 样品3 2.37 1.7 2.08 1.0 6.5
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