Determination of 34 Elements in Ground Substrate of Black Soil by ICP-MS/OES with Alkali Melting Digestion
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摘要:
黑土样品中有机质含量较高，通常在3%～10%之间，采用敞口酸溶、微波酸溶、高压密闭酸溶、灰化法等传统的前处理方法并不能将样品完全消解，而不同的元素需要采用不同的消解和测定方法，导致实验耗时长，操作过程复杂，分析成本过高，不适合多种元素同时测定。本文采用碳酸钠、四硼酸锂和偏硼酸锂作为混合熔剂分解样品，并提出在酸提取剂中加入酒石酸的方法来提取样品，利用电感耦合等离子体质谱法和发射光谱法(ICP-MS/OES)对黑土地地表基质中34种元素进行测定，解决了传统分析方法不适合多元素同时测定和钽铪等元素易水解的问题。研究了不同提取体系对钽铪元素提取效果的影响，确定了提取剂为30mL盐酸−10mL 100g/L酒石酸是最佳比例。方法检出限为0.01～50.13μg/g，测定结果能够满足土壤分析要求。采用不同种类的土壤标准物质对本方法进行验证，各元素的测定值与标准值基本一致，相对标准偏差(RSD)为0.48%～4.53%，相对误差(RE)为−5.23%～4.85%，实际样品分析的相对标准偏差均在0.16%～4.97%之间。
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关键词:
- 电感耦合等离子体质谱法 /
- 电感耦合等离子体发射光谱法 /
- 酒石酸 /
- 碱熔 /
- 黑土
Abstract:The organic matter content in black soil samples is high, typically ranging from 3% to 10%. Traditional pretreatment methods such as open acid dissolution digestion, microwave acid dissolution and digestion, high-pressure closed acid dissolution and digestion, and ashing method cannot completely digest the sample, and different elements need to adopt different digestion and determination methods, resulting in long experiments, complex operation processes, high analysis costs, and are not suitable for the simultaneous determination of multiple elements. Sodium carbonate, lithium tetraborate and lithium metaborate were selected as mixed fluxes to digest the samples, and a method of adding tartaric acid to the acid extractor was proposed to extract the samples. 34 elements in the ground substrate of black soil were determined by inductively coupled plasma-mass spectrometry/optical emission spectrometry (ICP-MS/OES). The traditional black soil sample analysis method is not suitable for the simultaneous determination of multiple elements and the easy hydrolysis of elements such as tantalum and hafnium, while ICP-MS/OES is suitable. The effects of different extraction systems on the extraction of tantalum and hafnium were studied, and the optimal ratio of 30mL of hydrochloric acid and 10mL of 100g/L tartaric acid was determined. On this basis, the detection limit of the samples was 0.010−50.13μg/g by the experimental method of control samples, and the results satisfied the requirements of soil analysis and detection. At the same time, different kinds of soil reference materials were selected for practical testing, and the measured values of each element were basically consistent with the standard values, with the relative standard deviations (RSDs) between 0.48%−4.53% and the relative errors between −5.23%−4.85%. In addition, to further verify the feasibility of the method, the relative standard deviations were all between 0.16%−4.97% when applied to actual samples.
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表 1 标准溶液系列浓度
Table 1. Different concentrations of standard solution series
混合标准储备
溶液编号待测元素 浓度 混标1 Bi，Co，La，Ce，Pr，Nd，
Sm，Eu，Gd，Tb，Dy，Ho，
Er，Tm，Yb，Lu，Y，Ta，
Hf，W，Mo，Th，Tl，U0，1，2，5，10，
20，50μg/L混标2 Mn，Ti，Ba，Sr 0，0.1，1，2，5，
10，20mg/L混标3 K，Na，Ca，Mg，Al，Fe 0，1，10，20，50，
100，200mg/L
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表 2 不同提取体系中土壤标准物质钽、铪元素的测定结果
Table 2. Analytical results of Ta and Hf in soil reference materials with different extraction systems
标准物质
编号Ta含量(μg/g) Hf含量(μg/g) 标准值 40mL盐酸
测定值盐酸-酒石酸体积比 标准值 40mL盐酸
测定值盐酸-酒石酸体积比 3∶1 1∶1 1∶3 3∶1 1∶1 1∶3 GBW07978 1.26 0.99 1.24 1.16 1.11 8.3 7.01 8.21 8.0 7.9 GBW07979 1.27 1.03 1.26 1.19 1.15 7.3 6.35 7.23 6.96 6.82 GBW07980 2.63 2.01 2.55 2.45 2.36 7.9 6.15 7.83 7.66 7.45
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表 3 线性回归方程、相关系数和方法检出限
Table 3. Linear regression equation, correlation coefficient and detection limit of the method
测定方法 元素 线性范围
(mg/L)线性回归方程 相关系数
(R2)方法检出限
(μg/g)ICP-MS Bi 0.1 y=40.351x+0.239 0.9998 0.10 Co 0.1 y=0.015x−0.0055 0.9996 0.03 La 0.1 y=0.0471x−0.102 0.9999 0.10 Ce 0.1 y=0.0505x−0.1016 0.9999 0.06 Pr 0.1 y=0.0741x−0.1802 0.9999 0.01 Nd 0.1 y=0.0272x−0.0517 0.9999 0.02 Sm 0.1 y=0.0259x−0.1029 0.9997 0.02 Eu 0.1 y=0.0513x−0.028 0.9998 0.01 Gd 0.1 y=0.0236x+0.0011 0.9998 0.02 Tb 0.1 y=0.1101x−0.3521 0.9999 0.01 Dy 0.1 y=0.0328x+0.0183 0.9997 0.02 Ho 0.1 y=0.1182x−0.4174 0.9999 0.01 Er 0.1 y=0.0395x+0.0808 0.9999 0.01 Tm 0.1 y=0.121x−0.0324 0.9997 0.02 Yb 0.1 y=0.0429x+0.0003 0.9999 0.01 Lu 0.1 y=0.1457x−0.5858 0.9999 0.01 Y 0.1 y=0.0347x+0.0356 0.9998 0.06 Ta 0.1 y=0.0347x+0.0356 0.9998 0.01 Hf 0.1 y=0.0003x+1.26×10−6 0.9998 0.03 W 0.1 y=95.71x+1.0292 0.9998 0.21 Mo 0.1 y=0.0227x−0.0021 0.9999 0.02 Th 0.1 y=0.086x−0.0021 0.9993 0.02 Tl 0.1 y=0.0451x−0.0121 0.9997 0.01 U 0.1 y=0.1328x−0.0523 0.9995 0.03 ICP-OES Al2O3 100 y=7.484x+198.657 0.9996 41.04 TFe2O3 100 y=327.867x+47.898 0.9998 37.59 MgO 100 y=139249.452x+31935.310 0.9993 4.74 CaO 100 y=3914.427x+2990.342 0.9992 17.76 Na2O 100 y=327.867x+47.898 0.9998 50.13 K2O 100 y=1875.342x+2452.084 0.9994 38.52 Mn 10 y=34.057x+459.306 0.9994 1.32 Ti 10 y=37.370x−644.631 0.9994 2.46 Ba 10 y=541247.043x+1325.417 0.9998 0.63 Sr 10 y=11023.809x+670.300 0.9998 0.15
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表 4 方法精密度和准确度测试结果
Table 4. Precision and accuracy tests of the method
元素 GBW07978 GBW07979 GBW07980 标准值
(μg/g)测定值
(μg/g)相对误差
(%)RSD
(%)标准值
(μg/g)测定值
(μg/g)相对误差
(%)RSD
(%)标准值
(μg/g)测定值
(μg/g)相对误差
(%)RSD
(%)Bi 0.38 0.37 −1.70 1.72 0.31 0.30 −4.81 2.91 301 301.66 0.22 1.14 Co 16 16.33 2.09 1.7 15.5 15.57 0.47 1.10 9.5 9.63 1.40 1.43 La 41 39.68 −3.22 0.86 37 37.48 1.29 0.90 55 57.52 4.58 1.18 Ce 82 80.74 −1.54 1.23 70 72.83 4.04 1.01 111 115.20 3.78 0.76 Pr 9.6 9.36 −2.47 1.08 8.5 8.44 −0.76 1.22 12.5 13.02 4.15 1.21 Nd 37 35.07 −5.23 1.53 33.2 34.04 2.54 0.56 45.9 47.05 2.51 0.94 Sm 7.1 7.12 0.22 2.14 6.3 6.27 −0.41 0.96 9.0 9.06 0.62 0.99 Eu 1.4 1.39 −0.86 1.56 1.4 1.41 0.60 1.37 1.27 1.23 −3.44 1.63 Gd 6.2 6.14 −0.92 1.32 5.8 5.99 3.35 1.72 8.0 8.06 1.07 1.17 Tb 1 1.03 2.51 2.03 0.94 0.91 −3.41 1.87 1.34 1.39 3.39 2.50 Dy 5.6 5.65 0.84 0.48 5.2 5.24 0.84 1.45 7.8 7.86 0.78 1.38 Ho 1.12 1.10 −1.78 1.51 1.04 1.05 1.16 1.64 1.55 1.57 1.33 0.97 Er 3.2 3.06 −4.39 1.95 2.9 2.95 1.80 0.73 4.6 4.82 4.8 1.14 Tm 0.51 0.52 2.57 1.37 0.46 0.47 2.27 2.34 0.75 0.77 2.09 1.17 Yb 3.2 3.35 4.80 1.78 2.9 2.94 1.30 1.17 5.1 5.06 −0.69 1.14 Lu 0.5 0.51 2.51 0.96 0.43 0.44 2.83 1.72 0.78 0.78 0.14 1.94 Y 29.9 30.05 0.51 0.78 28.6 28.63 0.12 1.08 43.7 45.49 4.09 1.11 Ta 1.26 1.27 0.57 1.88 1.27 1.26 −1.17 0.94 2.63 2.65 0.89 1.03 Hf 8.3 8.08 −2.65 1.20 7.3 7.23 −0.92 1.5 7.9 8.03 1.61 1.48 W 2.1 2.20 4.85 1.02 1.8 1.82 1.31 1.54 164 156.9 −4.33 1.38 Mo 0.68 0.65 −3.80 3.81 1.11 1.11 0.03 2.49 12.2 12.79 4.83 1.14 Th 13.6 13.53 −0.55 1.82 11.2 11.2 −1.05 1.30 23.9 24.58 2.83 0.99 Tl 0.73 0.74 1.96 1.56 0.58 0.60 4.50 1.69 2.13 2.11 −1.02 1.13 U 3.1 3.05 −1.68 1.43 2.1 2.08 −1.11 1.17 15.6 15.36 −1.55 0.85 Al2O3 148400 143880 −3.05 1.27 132100 135064 2.24 1.71 127000 128578 1.24 0.79 TFe2O3 51300 53188 3.68 2.93 49800 49198 −1.21 4.36 82900 85404 3.02 2.18 MgO 12400 11998 −3.24 3.21 20700 21485 3.79 3.89 9200 9441 2.62 1.76 CaO 13900 14023 0.88 1.69 21800 22191 1.79 1.68 11800 12137 2.86 1.89 Na2O 17300 17840 3.12 2.98 19500 20206 3.62 4.53 1300 1335 2.69 3.56 K2O 27200 27411 0.78 2.00 25100 25720 2.47 2.84 18300 17964 −1.84 2.05 Mn 923 908 −1.60 2.35 674 660 −2.38 1.48 1675 1740 3.86 2.47 Ti 4760 4742 −0.37 2.13 4570 4616 1.00 1.98 4100 4138 0.93 1.17 Ba 639 641 0.38 3.17 679 674 −0.79 4.28 255 248 −2.71 3.49 Sr 186 182 −2.40 2.51 151 154 1.82 2.70 26.3 26.45 0.55 1.69
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表 5 黑土地地表基质样品中34种元素分析结果(n=10)
Table 5. Analytical results of 34 elements in ground substrate samples of black soil (n=10)
元素 实际样品S1 实际样品S2 实际样品S3 元素 实际样品S1 实际样品S2 实际样品S3 测定值
(μg/g)RSD
(%)测定值
(μg/g)RSD
(%)测定值
(μg/g)RSD
(%)测定值
(μg/g)RSD
(%)测定值
(μg/g)RSD
(%)测定值
(μg/g)RSD
(%)Bi 2.89 0.16 0.24 3.74 0.17 2.36 Ta 0.91 2.19 1.08 2.13 1.57 1.17 Co 11.16 1.19 13.64 1.52 11.45 1.46 Hf 9.13 1.46 6.87 2.09 6.73 1.66 La 21.57 1.37 26.71 2.17 25.24 1.86 W 0.87 3.62 1.28 2.00 1.08 1.57 Ce 40.74 1.55 50.85 1.57 47.67 1.82 Mo 0.38 4.97 0.52 3.61 0.78 2.77 Pr 4.66 2.17 5.75 2.35 5.57 2.54 Th 5.48 2.42 8.90 1.10 6.17 1.62 Nd 17.39 1.37 21.03 2.00 20.67 1.32 Tl 0.40 2.49 0.55 1.92 0.46 2.70 Sm 3.05 2.55 3.75 1.93 3.86 2.28 U 1.36 2.00 1.58 2.00 2.52 1.63 Eu 0.70 2.40 0.83 1.63 0.86 2.20 Al2O3 130291 1.57 131927 1.40 135236 1.15 Gd 3.17 2.17 3.75 2.85 3.88 2.38 TFe2O3 52914 3.72 57903 2.55 47205 3.30 Tb 0.44 3.67 0.55 1.26 0.57 4.56 MgO 10160 3.26 11095 2.95 11263 2.11 Dy 2.38 2.26 3.20 2.18 3.17 2.25 CaO 9997 3.65 9990 2.61 11334 2.14 Ho 0.48 2.25 0.65 1.83 0.62 2.26 Na2O 17326 3.97 17783 2.7 20010 3.49 Er 1.31 1.99 1.83 2.03 1.72 2.46 K2O 28325 3.2 27825 2.35 29015 1.91 Tm 0.20 3.15 0.29 2.22 0.27 1.92 Mn 1792 2.46 1134 2.29 2605 2.66 Yb 1.31 1.77 1.92 1.70 1.72 1.93 Ti 5331 1.58 5676 2.02 5905 1.84 Lu 0.21 1.35 0.30 2.01 0.26 2.28 Ba 863 2.52 686 2.53 968 2.95 Y 16.56 1.42 22.72 1.62 21.92 1.74 Sr 143 1.73 140 2.59 197 2.21
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表 6 实际样品采用不同消解方法34种元素分析结果
Table 6. Analytical results of 34 elements in actual samples with different digestion methods
元素 实际样品S4 实际样品S5 元素 实际样品S4 实际样品S5 本方法(碱熔法)
测定值(μg/g)封闭酸溶法
测定值(μg/g)本方法(碱熔法)
测定值(μg/g)封闭酸溶法
测定值(μg/g)本方法(碱熔法)
测定值(μg/g)封闭酸溶法
测定值(μg/g)本方法(碱熔法)
测定值(μg/g)封闭酸溶法
测定值(μg/g)Ta 0.542 0.577 8.3 7.01 Gd 2.005 2.089 6.004 5.818 Hf 5.483 5.964 7.9 6.15 Tb 0.351 0.345 0.958 0.881 La 13.19 13.59 45.48 44.81 Dy 1.846 1.974 5.697 5.351 Ce 23.88 25.39 86.46 84.29 Ho 0.403 0.424 1.108 1.051 Pr 3.169 3.358 9.75 9.554 Er 1.151 1.214 3.219 3.154 Nd 12.59 13.02 37.07 36.31 Tm 0.203 0.21 0.504 0.499 Sm 2.334 2.46 6.89 6.731 Yb 1.345 1.379 3.182 3.185 Eu 0.588 0.633 1.31 1.269 Lu 0.213 0.234 0.499 0.485
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