Simultaneous Determination of 48 Elements in Marine Sediments by ICP-MS with Lithium Metaborate Fusion
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摘要:
海洋沉积物常用的分析方法如敞开消解或高压密闭消解结合电感耦合等离子体质谱（ICP-MS）或电感耦合等离子体发射光谱（ICP-OES）测定，粉末压片或熔片结合X射线荧光光谱法（XRF）测定，分别存在消解不完全、速度慢、检出限高等缺点，导致样品前处理效率低、待测元素少。针对上述问题，本文采用偏硼酸锂为熔剂分解样品，5%硝酸浸取，用ICP-MS法进行测定，建立了一种快速分析海洋沉积物中48种元素的方法。使用海洋沉积物国家标准物质作为高点绘制标准工作曲线，确定了助熔剂偏硼酸锂用量、稀释倍数、各待测元素的分析同位素及内标元素、仪器测定模式及个别元素的干扰校正方程等，得到最佳分解条件及测定条件。结果表明：由于高温损失，P、As、Se、Cd、Hg等元素无法得到准确结果，可改用微波消解等方式前处理后再进行测定；Cu、Zn、Cr、Ni、Co等共计48种元素使用本法均能得到准确结果，各元素方法精密度（RSD）均小于9.7%。本方法应用于分析海洋沉积物国家标准物质GBW07333、GBW07314、GBW07335、GBW07336，测定值和认定值相符；分析海洋沉积物实际样品，各元素加标回收率介于83.6%~118.6%。本方法可测定元素多，极大提高了分析效率，适合大批量样品分析。
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关键词:
- 海洋沉积物 /
- 碱熔 /
- 偏硼酸锂 /
- 电感耦合等离子体质谱法
Abstract:BACKGROUND The common analysis methods of marine sediments, such as open digestion or high-pressure closed digestion combined with inductively coupled plasma-mass spectrometry (ICP-MS) or inductively coupled plasma-optical emission spectroscopy (ICP-OES) determination, and pressed powder pellet or fusion tablets combined with XRF determination, have a low efficiency of sample pretreatment and less detectable elements. The disadvantages of incomplete digestion, slow speed and high detection limit contribute to the inefficiency of the method.
OBJECTIVES To develop a rapid method for the determination of 48 elements in marine sediments by ICP-MS.
METHODS Lithium metaborate was used as a flux to decompose the sample. The obtained sample was leached with 5% nitric acid and determined by ICP-MS. An analytical method for the rapid determination of 48 elements in marine sediments was established. Using the national standard references materials of marine sediment as the high point, the standard working curve was drawn. The amount of flux LiBO2, dilution ratio, analytical isotope and internal standard elements of each element to be measured, instrument measurement mode and interference correction equation of individual elements were determined, an optimal decomposition conditions and measurement conditions were obtained.
RESULTS The results showed that the accurate results of P, As, Se, Cd, Hg cannot be obtained due to high temperature loss, yet microwave digestion or other methods could be used for pretreatment to avoid loss before determination. The accurate results of 48 elements may be obtained by this method, the relative standard deviation (RSD) of each element was less than 9.7%. The measured values of the national standard references of marine sediments GBW07333, GBW07314, GBW07335 and GBW07336 were consistent with the certified values. The recoveries of each element in marine sediment samples ranged from 83.6% to 118.6%.
CONCLUSIONS This method greatly improves the analysis efficiency, and can analyze more elements, suitable for the analysis of large numbers of samples.
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表 1 不同偏硼酸锂加入量对GBW07314中难溶元素分析结果的影响
Table 1. Effect of different LiBO2 addition on analysis results of refractory elements in GBW07314
元素 认定值(μg/g) 测定值(μg/g) 0.200g偏硼酸锂 0.300g偏硼酸锂 0.400g偏硼酸锂 0.500g偏硼酸锂 Zr 229 111 172 225 209 Hf 6.2 2.74 3.04 6.41 6.80 Nb 19.1 4.25 6.83 18.6 17.2 Ta 1.2 0.436 0.702 1.23 1.38 W 2.1 1.24 1.69 2.02 2.14 Mo 0.64 0.177 0.415 0.603 0.612 
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表 2 方法检出限
Table 2. Detection limit of the method
待测元素 检出限(μg/g) 待测元素 检出限(μg/g) Cu 1.479 Tm 0.006 Zn 11.452 Rb 0.549 Cr 16.262 Sc 0.330 Ni 0.995 Th 0.067 Co 0.236 V 1.168 Pb 2.955 Nb 0.137 Sr 0.357 Ta 0.067 Ba 3.616 Hf 0.021 Ga 0.466 Cs 0.043 Mo 0.113 W 0.064 Zr 0.360 Sb 0.051 La 0.391 U 0.098 Ce 0.157 Tb 0.015 Nd 0.267 Bi 1.096 Sm 0.064 Be 0.430 Eu 0.008 SiO2* 0.870 Ho 0.007 Al2O3* 0.026 Yb 0.074 Fe2O3* 0.033 Lu 0.006 CaO* 0.051 Y 0.442 MgO* 0.004 Pr 0.025 K2O* 0.192 Gd 0.077 Na2O* 0.080 Dy 0.026 MnO* 0.001 Er 0.113 TiO2* 0.001 注：标注“*”的待测元素检出限单位为%。
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表 3 国家标准物质测定结果及加标回收率
Table 3. Analytical results of national standard references and their spiked recovery
待测元素 GBW07314 GBW07333 GBW07335 GBW07336 回收率(%) 认定值(μg/g) 测定值(μg/g) 认定值(μg/g) 测定值(μg/g) 认定值(μg/g) 测定值(μg/g) 认定值(μg/g) 测定值(μg/g) Cu 31 29.9 29.1 26.5 18 16.6 23 20.8 96.2 Zn 87 85.5 114 112 79 75.4 100 95.5 91.4 Cr 86 77.8 107 98.5 78 73.9 64 57.9 91.4 Ni 34.3 32.7 46.1 42.0 36 35.7 44 42.5 87.8 Co 14.2 13.3 18.9 18.6 15 14.9 13 12.3 83.6 Pb 25 23.6 29 26.9 25 23.5 20 18.3 92.2 Sr 150 142 130 124 193 184 507 463 96.0 Ba 425 424 477 449 396 361 488 479 96.4 Ga 16.1 16.0 - 19.2 16 14.8 15.1 14.1 114.6 Mo 0.64 0.651 - 0.462 - 1.42 - 1.08 107.8 Zr 229 227 144 132 184 171 134 128 105.2 La 38 35.6 40.8 39.9 38 36.0 31 28.0 93.6 Ce 78 70.4 77.4 75.9 78 71.5 64 62.8 86.6 Nd 33 30.0 33.1 31.6 32.6 30.2 26 25.0 112.0 Sm 6.7 6.48 6.28 6.18 6.2 6.03 5.2 4.77 89.8 Eu 1.3 1.24 1.26 1.16 1.25 1.24 1.01 0.93 91.2 Ho 1 0.965 0.96 0.952 0.92 0.839 0.8 0.744 110.0 Yb 2.8 2.61 2.46 2.23 2.42 2.21 2.2 2.11 85.2 Lu 0.45 0.425 0.37 0.355 0.38 0.374 0.31 0.318 86.2 Y 27 25.2 24.9 23.7 25 25.0 23 20.7 109.4 Pr 8.7 7.98 8.32 7.51 8.3 7.59 6.8 6.26 85.2 Gd 5.6 5.46 5.44 4.98 5.4 5.09 4.5 4.08 86.2 Dy 5.4 5.18 4.59 4.43 4.8 4.74 4.1 3.97 107.2 Er 3 2.94 2.57 2.49 2.56 2.42 2.3 2.09 108.8 Tm 0.44 0.442 0.38 0.355 0.39 0.364 0.29 0.285 109.6 Rb 109.3 104 164 164 118 113 110 99.8 95.0 Sc 12.5 11.6 16.1 15.1 12 11.9 11 10.8 118.6 Th 10.2 9.52 14.2 13.2 13.6 12.6 12.6 12.0 93.4 V 103.1 95.5 131 128 95 91.3 87 85.6 109.6 Nb 19.1 18.3 17.1 16.3 13.7 13.2 12.9 12.4 116.5 Ta 1.2 1.08 1.22 1.21 - 1.62 - 1.08 110.0 Hf 6.2 6.09 5.2 4.83 5 4.91 5 4.80 97.2 Cs 8.2 8.11 13.8 13.4 8 7.33 7.6 7.28 105.6 W 2.1 1.97 1.93 1.82 - 2.11 - 1.97 104.8 Sb 1.4 1.39 1.06 0.972 - 0.865 - 1.32 96.0 U 2.7 2.66 4.5 4.45 2.7 2.61 2.8 2.54 113.2 Tb 0.83 0.821 0.76 0.725 0.8 0.762 0.7 0.645 107.8 Be - 2.42 - 1.61 - 1.72 - 1.71 99.2 Bi - 0.621 0.45 0.431 - 0.515 - 1.46 110.2 SiO2* 61.91 60.4 54 51.3 59.6 55.3 44.9 44.4 - Al2O3* 13.07 12.58 17.42 17.32 13.1 12.06 12.1 11.9 96.2 Fe2O3* 5.36 5.14 6.77 6.17 5.28 5.23 4.65 4.57 91.0 CaO* 4.31 4.27 1.47 1.34 4.8 4.51 4.8 4.62 112.5 MgO* 2.5 2.43 3.08 2.84 2.51 2.4 2.51 2.31 87.5 K2O* 2.48 2.44 3.53 3.36 2.71 2.63 2.71 2.65 93.5 Na2O* 1.68 1.53 2.93 2.66 2.3 2.12 2.5 2.37 103.0 MnO* 0.096 0.112 0.062 0.0641 0.073 0.0754 0.3 0.274 109.9 TiO2* 0.825 0.824 0.775 0.711 0.72 0.654 0.61 0.595 101.2 注：标注“*”的待测元素认定值和测定值的数据单位为%。
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