Development of Separating and Purifying Methods for Lithium Isotope Analysis of Bauxite
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摘要: 铝土矿是极端风化作用的产物，也是锂的重要载体，由于其资源量巨大，对铝土矿中锂的富集机制和分布规律的研究将有利于找矿预测。锂同位素的高效准确分析是深入认识矿物中锂的富集机制和分布规律的基础。铝土矿样品由于化学稳定性较强，溶样过程较为复杂，且Al、Na、Ca、K等基体元素含量远高于锂，给锂的纯化增加不少难度。本文采用内径5mm、柱长190mm的聚四氟乙烯离子交换柱和AG50W-X12阳离子交换树脂，以0.5mol/L硝酸为淋洗液淋洗34mL，收集最后的12mL，即可完成对铝土矿中锂的完全纯化回收。该纯化方法减少了淋洗液的使用量，提高了实验效率。采用该方法对国际标样L-SVEC、RGM-2、GSP-2进行锂的纯化，通过多接收电感耦合等离子体质谱仪（MC-ICP-MS）测试锂同位素组成，得到的δ7Li测试值分别为－0.26‰±0.09‰（2SD，n=3）、3.19‰±0.37‰（2SD，n=3）、－0.78‰±0.22‰（2SD，n=3），与前人报道一致，验证了该方法的可靠性。此外，采用本方案对铝土矿国家标样（GBW07182）进行锂的纯化，δ7Li测定值为10.16‰±0.21‰（2SD，n=3）。Abstract:
BACKGROUNDBauxite is a product from extreme weathering, an important carrier of lithium. Due to its huge resources, the study on the mechanism and distribution of lithium in bauxite will be beneficial to the prospecting and prediction of bauxite deposits. Efficient and accurate analysis of lithium isotopes is the basis for deep understanding of the lithium enrichment mechanism and distribution driplines in the ores. The bauxite samples are more chemically stable and the sample dissolution process is more complicated. The content of matrix elements such as Al, Na, Ca and K is much higher than that of Li, which makes it difficult to purify Li. OBJECTIVESTo establish a method for separating and purifying lithium in bauxite for Li isotope analysis. METHODSOn the basis of previous studies, the separation, purification, and measurement scheme of Li in bauxite were investigated by leaching experiment. RESULTSIn this scheme, polytetrafluoroethylene exchange column with an inner diameter of 5mm and a column length of 190mm, and AG50W-X12 cation exchange resin were used. 34mL of 0.5mol/L nitric acid was used as the eluent and the final solution was 12mL, resulting in complete purification and recovery of Li in bauxite. At the same time, the method was used to purify the Li in international standard samples, L-SVEC, RGM-2 and GSP-2, and the values of δ7Li were measured by MC-ICP-MS, which were -0.26‰±0.09‰ (2SD, n=3), 3.19‰±0.37‰ (2SD, n=3), -0.78‰±0.22‰ (2SD, n=3). The analytical results were consistent with the previous results obtained by other methods, verifying the reliability of this method. The proposed method was used to purify bauxite standard sample, GBW07182, which yielded δ7Li of 10.16‰±0.21‰ (2SD, n=3). CONCLUSIONSThe purification method reduces the amount of eluent used and improves experimental efficiency. -
Key words:
- bauxite /
- associated lithium /
- separation and purification /
- Li isotope /
- MC-ICP-MS /
- standard materials
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表 1 测量离子浓度和锂同位素的仪器参数
Table 1. Instrument parameters for measuring ion concentration and Li isotope
仪器类型 参数 工作条件 ICP-MS
(型号Agilent 7900)射频功率 1550W 采样深度 8.00mm 雾化气流量 1.10L/min 雾化室温度 1℃ MC-ICP-MS
(型号Neptune Plus)射频功率 1200W 样品冷却气流量 15.00L/min 样品辅助气流量 0.70L/min 样品气流量 1.13L/min 提取电压 -2000V 仪器质量分辨率 低分辨 样品锥和截取锥 Jet sampler, X skimmer 杯 L4，C，H4 
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表 2 标样中锂元素含量
Table 2. Li element content in standard samples
标样编号 元素组成/成分 元素浓度
(μg/g)来源 Y-1 Li 1 阿法埃莎化学有限公司 Ag、Al、As、Ba、Cu、Cd、
Co、Cs、Fe、Ga、K、Mg、
Mn、Na、Rb、Zn、Ni、Se、
U、Pb、Sn、V各元素
浓度
均为1Y-2 Li 0.4 阿法埃莎化学有限公司 Na 2.0 Al 120.0 Mg 5.6 K 10.8 Ca 24.8 Ti 7.6 Fe 27.6 L-SVEC 纯碳酸锂 约100% 美国国家标准技术研究院 RGM-2 流纹岩 57 美国地质调查局 GSP-2 花岗闪长岩 36 美国地质调查局 GBW07182 铝土矿 147 国家地质实验测试中心 GSB Li Li 约100% 国家钢铁材料测试中心 Alfa Li Li 约100% 阿法埃莎化学有限公司
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表 3 不同锂分离提纯方法的对比
Table 3. Comparison of Li separation and purification methods
方法编号 分离提纯实验步骤 交换柱 参考文献 1 ①用6mL 0.5mol/L硝酸平衡树脂(2mL/次)。
②将样品蒸干后溶于1mL 0.5mol/L硝酸，注入柱子中。
③用0.5mol/L硝酸淋洗，收集22~34mL区间内的淋洗液。聚四氟乙烯交换柱
(内径5mm，柱长190mm)本文 2 ①用3倍于柱子体积的0.5mol/L盐酸平衡树脂。
②将样品蒸干后溶于200μL0.5mol/L盐酸，注入柱子中。
③用0.5mol/L盐酸淋洗，收集6~11mL区间内的淋洗液。聚四氟乙烯交换柱
(内径3.2mm，柱长250mm)[29] 3 ①用20mL 0.15mol/L盐酸分两次平衡柱子。
②将样品蒸干后溶于0.15mol/L盐酸，注入柱子中。
③用190mL 0.15mol/L盐酸淋洗，收集后面80mL淋洗液。石英交换柱
(内径8mm，柱长300mm)[6] 4 ①用1mL 4mol/L盐酸平衡柱子。
②将样品蒸干后溶于1mL 4mol/L盐酸，注入柱1。
③用5mL 2.8mol/L盐酸洗脱，收集1mL工作液和5mL淋洗液。聚丙烯交换柱
(填充1.2mL树脂)[30] ④将经柱1处理的淋洗液蒸干，溶于2mL 0.15mol/L盐酸，注入柱2。
⑤用21mL 0.15mol/L盐酸洗脱，收集加入的21mL淋洗液。聚丙烯交换柱
(填充1.5mL树脂)⑥将经过柱2处理的1mL工作液注入柱3。
⑦用8mL 0.5mol/L盐酸和30%乙醇洗脱，收集并蒸干。石英交换柱
(填充1mL树脂)5 ①用2mL 0.67mol/L硝酸和30%甲醇混合溶液平衡树脂。
②将1mL样品溶液注入柱子中(200μL/次)。
③用1mol/L硝酸和80%甲醇混合液淋洗，收集10~25mL区间内的淋洗液。石英交换柱
(内径6mm，柱长215mm)[31]
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表 4 GBW07182一次/二次纯化效果对比
Table 4. Comparison of primary/secondary purification effect for GBW07182
元素 元素含量(ng/g) GBW07182-柱1 GBW07182-柱2 Li 212.95 196.01 Na 518.22 325.66 Mg 8.38 0.00 Al 1251.65 0.51 K 126.51 21.34 Ca 111.83 52.40 Fe 51.36 0.00
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表 5 纯化过程中标样锂回收率统计
Table 5. Statistics of recovery rate of Li in standard samples purification process
样品编号 锂上样量
(ng)锂接收量
(ng)锂回收率
(%)淋洗区间
(mL)L-SVEC-柱1 429.38 429.38 100.0 25~33 Y-1-柱1 844.86 844.86 100.0 25~33 GBW07182-柱1 428.92 425.90 99.30 25~33 GBW07182-柱2 392.11 392.03 99.98 25~33 Y-2-柱1 425.25 425.25 100.0 25~33 L-SVEC-柱1 1086.98 1086.98 100.0 23~31 L-SVEC-柱1 2251.11 2251.11 100.0 25~33 L-SVEC-柱2 2279.03 2275.08 99.83 25~33 GBW07182-柱1 2557.13 2557.13 100.0 25~33 GBW07182-柱2 2856.76 2854.17 99.91 25~33
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表 6 本实验标准样品的锂同位素组成测定结果与文献报道值的对比
Table 6. Comparison of Li isotopic ratio in this experiment and reported values in literatures
标准样品编号 δ7Li测定值
(2SD，‰)数据来源 L-SVEC
(纯碳酸锂)0±2.4 [49] 0.0±0.03 [50] 0.2±0.82 [39] 0.2±0.3(未过柱) [51] -0.3±0.3(过柱) [51] -0.26±0.09(n=3)(2遍柱) 本实验 -0.31±0.34(n=3)(2遍柱) 本实验 RGM-2
(流纹岩)2.75±0.15 [31] 3.19±0.37(n=3)(2遍柱) 本实验 2.26±0.14(n=3)(2遍柱) 本实验 2.44±0.85(n=3)(2遍柱) 本实验 2.22±1.02(n=3)(2遍柱) 本实验 GSP-2
(花岗闪长岩)-0.86±0.26 [51] -0.75±0.21 [51] -0.8±0.3 [52] -0.78±0.25 [31] -0.64±0.19(n=3)(2遍柱) 本实验 -0.78±0.22(n=3)(2遍柱) 本实验 GBW07182
(铝土矿)10.84±0.26(n=3)(2遍柱) 本实验 10.23±0.18(n=3)(2遍柱) 10.07±0.06(n=3)(2遍柱) 10.46±0.25(n=3)(2遍柱) 9.93±0.27(n=3)(2遍柱) 9.89±0.10(n=3)(2遍柱) 10.48±0.34(n=3)(2遍柱) 10.15±0.14(n=3)(2遍柱) 10.26±0.24(n=3)(2遍柱) 10.01±0.18(n=3)(2遍柱) 9.81±0.39(n=3)(2遍柱) 9.83±0.16(n=3)(2遍柱)
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