Simultaneous Determination of 28 Elements including Rare Earth Elements by ICP-MS with Five-Acid Dissolution
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摘要:
电感耦合等离子体质谱法（ICP-MS）测定大批量地质样品中的稀土和钴铪铟锰铌钽铊铬镉镓锗钒锡等金属元素，主要采用三酸或四酸溶解样品。由于地质样品组分复杂，稀土等金属元素含量低，各元素性质差异大，三酸或四酸溶样经常出现易挥发元素如钒铬镉镓锡的测定结果不稳定、镧铈镨钕等稀土元素溶解不完全的问题。本文在盐酸-硝酸-氢氟酸-高氯酸四酸基础上引入硫酸，形成盐酸-硝酸-氢氟酸-高氯酸-硫酸五酸溶样体系，用于水系沉积物、土壤和岩石等不同类型地质样品的一次敞口溶解，采用在线加入185Re和103Rh内标方式，建立了应用ICP-MS同时测定稀土等28种金属元素的方法。钒铬镉镓锡元素的准确度提高了1.4%~14.6%，镧和铈元素的准确度提高了0.2%~8.9%。该方法应用于分析水系沉积物、土壤、岩石标准物质（分别为GBW07301a、GBW07408、GBW07107），其测定值与认定值相一致，相对标准偏差（RSD）为1.14%~9.84%，准确度（△lgC）均≤0.1。该方法分析过程较简单，结果准确可靠，可满足测定大批量地质样品中稀土和钴铪铟锰铌钽等金属元素含量的要求。
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关键词:
- 地质样品 /
- 稀土元素 /
- 金属元素 /
- 五酸溶样 /
- 电感耦合等离子体质谱法
Abstract:BACKGROUND Three acids and four acids dissolution methods are the two main dissolution methods for determination of rare earth, cobalt, hafnium, indium, manganese, niobium, tantalum, thallium, chromium, cadmium, gallium, germanium, vanadium and tin in geological samples by inductively coupled plasma-mass spectrometry (ICP-MS). However, the composition of geological samples is complex, the content of rare earth and other metal elements is low, and the properties of each element are different, which makes the measurement results of volatile elements such as vanadium, chromium, cadmium, gallium and tin unstable, and rare earth elements such as lanthanum, cerium, praseodymium and neodymium are not completely dissolved by three acids or four acids.
OBJECTIVES To improve the four acids dissolution system for the determination of 28 elements including rare earth elements and rare metal elements.
METHODS The method of HCl-HNO3-HF-HClO4-H2SO4 was developed by addition of H2SO4 in the dissolution system of HCl-HNO3-HF-HClO4. A new analysis method has been developed for the certified reference material of stream sediment, soil and rock, and 28 elements including rare earth elements in samples were determined simultaneously by ICP-MS with 10ng/mL 103Rh and 185Re as the internal standard by on-line injections.
RESULTS The accuracy of volatile elements such as vanadium, chromium, cadmium, gallium and tin was improved by 1.4%-14.6%, and that of rare earth elements such as lanthanum and cerium was improved by 0.2%-8.9%. The certified reference materials of stream sediment (GBW07301a), soil (GBW07408) and rock (GBW07107) were analyzed to test the method. The determined values were in good agreement with the certified values. The standard deviations (RSD) of the method were 1.14%-9.84% and accuracy (△lgC) was not higher than 0.1.
CONCLUSIONS This method is rapid, simple, and accurate and can meet the requirements for determining the content of rare earth, cobalt, hafnium, indium, manganese, niobium, tantalum and other metal elements in large quantities of geological samples.
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表 1 四酸和五酸溶样对易挥发元素镉铬镓锡和钒的影响
Table 1. Effect of different acid systems on volatile element Cd, Cr, Ga, Sn and V determination
标准物质编号 溶样方法 Cd含量
(μg/g)Cr含量
(μg/g)Ga含量
(μg/g)Sn含量
(μg/g)V含量
(μg/g)四酸溶样 0.133 142 20.6 2.92 103 GBW07301a 五酸溶样 0.117 130 22.2 3.17 112 认定值 0.110 128 23.6 3.30 115 四酸溶样 0.148 44.6 11.9 1.8 63 GBW07365 五酸溶样 0.174 49.7 13.0 2.1 66 认定值 0.165 48.0 13.4 2.0 69 四酸溶样 0.121 63.6 12.4 2.66 73.9 GBW07408 五酸溶样 0.132 69.6 14.5 2.75 83.3 认定值 0.13 68 14.8 2.80 81.0 四酸溶样 0.142 78.5 16.5 3.06 95 GBW07452 五酸溶样 0.147 80.7 17.5 3.27 107 认定值 0.150 82.0 18.5 3.40 104 四酸溶样 0.063 90 22.0 1.71 83 GBW07107 五酸溶样 0.076 103 24.3 2.15 88 认定值 0.070 99 26.0 2.00 87 四酸溶样 0.115 131 15.7 0.70 274 GBW07122 五酸溶样 0.127 139 16.7 0.85 305 认定值 0.140 137 17.2 0.80 296 
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表 2 四酸和五酸溶样对稀土元素铈和镧的影响
Table 2. Effect of different acid systems on rare earth element Ce and La determination
标准物质编号 Ce含量(μg/g) La含量(μg/g) 四酸溶样 五酸溶样 认定值 四酸溶样 五酸溶样 认定值 GBW07301a 80.7 81.6 81 36.8 39.6 41 GBW07365 44.5 45.5 47 22.1 23.9 24 GBW07408 64.4 64.9 66 33.7 34.3 36 GBW07452 75.8 77.5 78 38.9 41.1 42 GBW07107 107 110 109 56.6 61.5 62 GBW07122 7.0 7.6 7.7 2.49 3.05 2.9
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表 3 元素钡对铕和钕的影响
Table 3. Effect of Ba on Eu and Nd determination
标准物质编号 Ba含量(μg/g) Eu含量(μg/g) Nd含量(μg/g) 四酸溶样 五酸溶样 认定值 四酸溶样 五酸溶样 认定值 四酸溶样 五酸溶样 认定值 GBW07301a 938 386 920 1.54 1.68 1.70 33.6 36.1 36.0 GBW07365 596 231 584 0.88 1.05 1.08 20 21.1 23 GBW07408 493 198 480 1.02 1.24 1.20 26.3 28.2 32.0 GBW07452 456 210 441 1.25 1.51 1.40 34.1 35.2 36.0 GBW07107 456 269 450 1.53 1.87 1.70 43.1 49.1 48.0 GBW07122 60 37 62 0.83 0.85 0.91 6.16 6.38 6.50
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表 4 国家一级标准物质工作曲线测定结果
Table 4. Analytical results of elements in standard curve
元素 GBW07305a GBW07309 GBW07457 平均值
(μg/g)认定值
(μg/g)平均值
(μg/g)认定值
(μg/g)平均值
(μg/g)认定值
(μg/g)111Cd 0.252 0.26 0.95 0.9 0.539 0.52 140Ce 78.1 78 87.4 90 105 107 59Co 14.50 14.4 15.3 16 19.04 18.2 52Cr 83.7 85 68.7 70 91.3 94 163Dy 5.24 5.1 5.60 5.3 6.53 6.3 166Er 2.95 2.8 3.3 3 4.03 3.7 153Eu 1.36 1.33 1.22 1.3 1.414 1.38 69Ga 13.8 14 15.55 15.2 22.7 25 157Gd 5.48 5.5 6.20 5.9 6.57 6.6 72Ge 1.36 1.3 1.59 1.48 1.86 1.83 178Hf 9.40 9.7 10.15 9.7 6.23 6.4 165Ho 0.99 0.96 1.083 1.05 1.251 1.27 115In 0.06 0.056 0.0637 0.061 0.114 0.122 139La 39.1 40 42.5 44 48.1 50 175Lu 0.46 0.45 0.53 0.5 0.635 0.59 55Mn 628.1 620 1020 1010 1158 1120 93Nb 17.9 18 18.3 20 20.13 19.6 146Nd 34.3 34 34.1 36 41.6 43 141Pr 9.15 9.2 9.10 9.9 10.6 11 147Sm 6.38 6.3 6.19 6.6 7.40 7.4 118Sn 2.70 2.6 4.3 4 8.39 8.7 181Ta 1.26 1.3 1.36 1.38 1.82 1.8 159Tb 0.88 0.87 0.917 0.92 1.064 1.11 205Tl 0.47 0.49 1.21 1.28 1.31 1.2 169Tm 0.45 0.44 0.51 0.5 0.59 0.6 51V 101.9 97 103.3 99 129 124 89Y 26.3 27 28.2 29 31.5 34 172Yb 2.94 2.8 3.39 3.2 4.97 4.8
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