功能纤维的稀土富集性能及其在ICP光谱分析中的应用研究
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摘要
综述了国内外对稀土元素分离富集方法的现状及进展。根据离子交换纤维分子结构中所含的特殊功能基团,在合适的条件下能选择性地吸附某些金属离子,使它们与其它元素的离子实现分离的特性,并结合电感耦合等离子体原子发射光谱法(ICP-AES)的应用,研究了聚丙烯(PP)基强酸性阳离子交换纤维、聚丙烯(PP)基弱酸性阳离子交换纤维和聚丙烯腈(PAN)两性离子交换纤维作为离子交换剂,分离富集各种基体中的痕量La、Nd、Eu、Gd、Er和Yb等稀土元素。
1研究了聚丙烯(PP)基强酸性阳离子交换纤维富集稀土元素的条件。pH=3的含稀土待富集液,在上柱流速小于14 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 130 mg·g~(-1),Nd 142 mg·g~(-1),Eu 122 mg·g~(-1),Gd 151 mg·g~(-1),Er 104 mg·g~(-1),Yb 134 mg·g~(-1)。用10 mL 2.5 mol·L~(-1)的HNO_3可将被吸附的稀土完全洗脱。在洗脱前用0.5 mol·L~(-1)HNO_3预淋洗,可将大部分K、Na、Mg、Ca、Ba、Cu、Zn、Fe和Al等共存元素除去,而不影响稀土元素的回收率。该方法检出限为La 0.016 ng·mL~(-1),Nd 0.051 ng·mL~(-1),Eu0.006 ng·mL~(-1),Gd 0.029 ng·mL~(-1),Er 0.048 ng·mL~(-1),Yb 0.006 ng·mL~(-1),回收率为94.5%～103%,RSD 0.7%～5.2%。测定了水样,人工合成样,国家标准物质GSD-11及柑桔叶中的稀土元素,得到满意的结果。
2研究了聚丙烯(PP)基弱酸性阳离子交换纤维富集稀土元素的条件。pH=5的含稀土待富集液,在上柱流速小于10 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 86.5 mg·g~(-1),Nd 98.2 mg·g~(-1),Eu 98.7 mg·g~(-1),Gd 99.2 mg·g~(-1),Er 84.9 mg·g~(-1),Yb 91.5 mg·g~(-1)。用10 mL 1.0 mol·L~(-1)的HCl能很好地洗脱交换柱上的痕量稀土元素。该法能很好地富集水样,人工合成锌,钠和钡等基体样品中的痕量稀土。该方法检出限为La 0.015 ng·mL~(-1),Nd 0.039 ng·mL~(-1),Eu 0.0090 ng·mL~(-1),Gd 0.030 ng·mL~(-1),Er 0.015 ng·mL~(-1),Yb 0.0090 ng·mL~(-1),回收率为91.8%～103%,RSD 0.3%～5.6%。
3研究了聚丙烯腈(PAN)两性离子交换纤维富集痕量稀土元素的条件。pH=5含稀土待富集液,在上柱流速小于8 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 7.32 mg·g~(-1),Nd 7.61 mg·g~(-1),Eu 8.04 mg·g~(-1),Gd 7.95 mg·g~(-1),Er 9.12 mg·g~(-1),Yb 8.49 mg·g~(-1)。用10 mL 1.5 mol·L~(-1)的HNO_3能很好地洗脱交换柱上的痕量稀土元素。该法能很好地富集水样,人工合成锌,铜和钠等基体样品中的痕量稀土。该方法检出限为La 0.032 ng·mL~(-1),Nd 0.068 ng·mL~(-1),Eu 0.033 ng·mL~(-1),Gd 0.053 ng·mL~(-1),Er 0.045 ng·mL~(-1),Yb 0.019 ng·mL~(-1),回收率为90.0%～101%,RSD为0.4%～5.3%。
In this paper,the current situation and progress on the methods of separation and enrichment of rare earth elements at home and abroad were reviewed.Based on the characteristic of absorption of some metal ion for separation from other ions under certain conditions by special functional groups in the molecule of exchange fiber,the separation and enrichment of trace rare earth elements La、Nd、Eu、Gd、Er and Yb from various matrix were investigated using polypropylene based strong acidic cation ion exchange fiber, polypropylene based weak acidic cation exchange fiber,and polyacrylonitrile based amphoteric ion exchange fiber respectively with ICP-AES.
1 A method of enrich trace rare earth elements by polypropylene based strong acid cation ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 3,rare earth elements was enriched quantitatively at the flow rate within 14 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 2.5 mol·L~(-1)HNO_3.The adsorption capacity were La 130 mg·g~(-1),Nd 142 mg·g~(-1),Eu 122 mg·g~(-1),Gd 151 mg·g~(-1),Er 104 mg·g~(-1),Yb 134 mg·g~(-1).The coexisting elements of K,Na,Mg,Ca, Ba,Cu,Zn,Fe and Al could be removed by pre-eluting with 0.5 mol·L~(-1)HNO_3. The detection limit of the method was La 0.016 ng·mL~(-1),Nd 0.051 ng·mL~(-1),Eu 0.006 ng·mL~(-1),Gd 0.029 ng·mL~(-1),Er 0.048 ng·mL~(-1),Yb 0.006 ng·mL~(-1),the recovery was in the range of 94.5%～103%,and the RSD was between 0.7%～5.2 %.The method was validated by the determination of trace rare earth elements in water,artificial samples,orange leaf,and GSD-11 samples.
2 A method of enrich trace rare earth elements by polypropylene based weak acid cation ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 5,rare earth elements was enriched quantitatively at the flow rate within 10 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 1.0 mol·L~(-1)HCl.The adsorption capacity were La 86.5 mg·g~(-1),Nd 98.2 mg·g~(-1),Eu 98.7 mg·g~(-1),Gd 99.2 mg·g~(-1),Er 84.9 mg·g~(-1),Yb 91.5 mg·g~(-1).The detection limit of the method was La 0.015 ng·mL~(-1),Nd 0.039 ng·mL~(-1),Eu 0.0090 ng·mL~(-1),Gd 0.030 ng·mL~(-1), Er 0.015 ng·mL~(-1),Yb 0.0090 ng·mL~(-1),the recovery was in the range of 91.8%-103%,and the RSD was between 0.3%～5.6%.The method was validated by the determination of trace rare earth elements in water and artificial samples.
3 A method of enrich trace rare earth elements by polyacrylonitrile based amphoteric ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 5,rare earth elements was enriched quantitatively at the flow rate within 8 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 1.5 mol·L~(-1)HNO_3.The adsorption capacity were La 7.32 mg·g~(-1),Nd 7.61 mg·g~(-1),Eu 8.04 mg·g~(-1),Gd 7.95 mg·g~(-1),Er 9.12 mg·g~(-1),Yb 8.49 mg·g~(-1).The detection limit of the method was La 0.032 ng·mL~(-1),Nd 0.068 ng·mL~(-1),Eu 0.033 ng·mL~(-1),Gd 0.053 ng·mL~(-1), Er 0.045 ng·mL~(-1),Yb 0.019 ng·mL~(-1),the recovery was in the range of 90.0%～101%,and the RSD was between 0.4%～5.3%.The method was validated by the determination of trace rare earth elements in water and artificial samples.
1研究了聚丙烯(PP)基强酸性阳离子交换纤维富集稀土元素的条件。pH=3的含稀土待富集液,在上柱流速小于14 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 130 mg·g~(-1),Nd 142 mg·g~(-1),Eu 122 mg·g~(-1),Gd 151 mg·g~(-1),Er 104 mg·g~(-1),Yb 134 mg·g~(-1)。用10 mL 2.5 mol·L~(-1)的HNO_3可将被吸附的稀土完全洗脱。在洗脱前用0.5 mol·L~(-1)HNO_3预淋洗,可将大部分K、Na、Mg、Ca、Ba、Cu、Zn、Fe和Al等共存元素除去,而不影响稀土元素的回收率。该方法检出限为La 0.016 ng·mL~(-1),Nd 0.051 ng·mL~(-1),Eu0.006 ng·mL~(-1),Gd 0.029 ng·mL~(-1),Er 0.048 ng·mL~(-1),Yb 0.006 ng·mL~(-1),回收率为94.5%～103%,RSD 0.7%～5.2%。测定了水样,人工合成样,国家标准物质GSD-11及柑桔叶中的稀土元素,得到满意的结果。
2研究了聚丙烯(PP)基弱酸性阳离子交换纤维富集稀土元素的条件。pH=5的含稀土待富集液,在上柱流速小于10 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 86.5 mg·g~(-1),Nd 98.2 mg·g~(-1),Eu 98.7 mg·g~(-1),Gd 99.2 mg·g~(-1),Er 84.9 mg·g~(-1),Yb 91.5 mg·g~(-1)。用10 mL 1.0 mol·L~(-1)的HCl能很好地洗脱交换柱上的痕量稀土元素。该法能很好地富集水样,人工合成锌,钠和钡等基体样品中的痕量稀土。该方法检出限为La 0.015 ng·mL~(-1),Nd 0.039 ng·mL~(-1),Eu 0.0090 ng·mL~(-1),Gd 0.030 ng·mL~(-1),Er 0.015 ng·mL~(-1),Yb 0.0090 ng·mL~(-1),回收率为91.8%～103%,RSD 0.3%～5.6%。
3研究了聚丙烯腈(PAN)两性离子交换纤维富集痕量稀土元素的条件。pH=5含稀土待富集液,在上柱流速小于8 mL·min~(-1)时,稀土元素被定量富集。其平衡吸附量分别为La 7.32 mg·g~(-1),Nd 7.61 mg·g~(-1),Eu 8.04 mg·g~(-1),Gd 7.95 mg·g~(-1),Er 9.12 mg·g~(-1),Yb 8.49 mg·g~(-1)。用10 mL 1.5 mol·L~(-1)的HNO_3能很好地洗脱交换柱上的痕量稀土元素。该法能很好地富集水样,人工合成锌,铜和钠等基体样品中的痕量稀土。该方法检出限为La 0.032 ng·mL~(-1),Nd 0.068 ng·mL~(-1),Eu 0.033 ng·mL~(-1),Gd 0.053 ng·mL~(-1),Er 0.045 ng·mL~(-1),Yb 0.019 ng·mL~(-1),回收率为90.0%～101%,RSD为0.4%～5.3%。
In this paper,the current situation and progress on the methods of separation and enrichment of rare earth elements at home and abroad were reviewed.Based on the characteristic of absorption of some metal ion for separation from other ions under certain conditions by special functional groups in the molecule of exchange fiber,the separation and enrichment of trace rare earth elements La、Nd、Eu、Gd、Er and Yb from various matrix were investigated using polypropylene based strong acidic cation ion exchange fiber, polypropylene based weak acidic cation exchange fiber,and polyacrylonitrile based amphoteric ion exchange fiber respectively with ICP-AES.
1 A method of enrich trace rare earth elements by polypropylene based strong acid cation ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 3,rare earth elements was enriched quantitatively at the flow rate within 14 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 2.5 mol·L~(-1)HNO_3.The adsorption capacity were La 130 mg·g~(-1),Nd 142 mg·g~(-1),Eu 122 mg·g~(-1),Gd 151 mg·g~(-1),Er 104 mg·g~(-1),Yb 134 mg·g~(-1).The coexisting elements of K,Na,Mg,Ca, Ba,Cu,Zn,Fe and Al could be removed by pre-eluting with 0.5 mol·L~(-1)HNO_3. The detection limit of the method was La 0.016 ng·mL~(-1),Nd 0.051 ng·mL~(-1),Eu 0.006 ng·mL~(-1),Gd 0.029 ng·mL~(-1),Er 0.048 ng·mL~(-1),Yb 0.006 ng·mL~(-1),the recovery was in the range of 94.5%～103%,and the RSD was between 0.7%～5.2 %.The method was validated by the determination of trace rare earth elements in water,artificial samples,orange leaf,and GSD-11 samples.
2 A method of enrich trace rare earth elements by polypropylene based weak acid cation ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 5,rare earth elements was enriched quantitatively at the flow rate within 10 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 1.0 mol·L~(-1)HCl.The adsorption capacity were La 86.5 mg·g~(-1),Nd 98.2 mg·g~(-1),Eu 98.7 mg·g~(-1),Gd 99.2 mg·g~(-1),Er 84.9 mg·g~(-1),Yb 91.5 mg·g~(-1).The detection limit of the method was La 0.015 ng·mL~(-1),Nd 0.039 ng·mL~(-1),Eu 0.0090 ng·mL~(-1),Gd 0.030 ng·mL~(-1), Er 0.015 ng·mL~(-1),Yb 0.0090 ng·mL~(-1),the recovery was in the range of 91.8%-103%,and the RSD was between 0.3%～5.6%.The method was validated by the determination of trace rare earth elements in water and artificial samples.
3 A method of enrich trace rare earth elements by polyacrylonitrile based amphoteric ion exchange fiber was studied.The conditions of enrichment and eluent were optimized.When the pH of pregnant solution was 5,rare earth elements was enriched quantitatively at the flow rate within 8 mL·min~(-1).Then it was desorbed from the column completely by 10 mL 1.5 mol·L~(-1)HNO_3.The adsorption capacity were La 7.32 mg·g~(-1),Nd 7.61 mg·g~(-1),Eu 8.04 mg·g~(-1),Gd 7.95 mg·g~(-1),Er 9.12 mg·g~(-1),Yb 8.49 mg·g~(-1).The detection limit of the method was La 0.032 ng·mL~(-1),Nd 0.068 ng·mL~(-1),Eu 0.033 ng·mL~(-1),Gd 0.053 ng·mL~(-1), Er 0.045 ng·mL~(-1),Yb 0.019 ng·mL~(-1),the recovery was in the range of 90.0%～101%,and the RSD was between 0.4%～5.3%.The method was validated by the determination of trace rare earth elements in water and artificial samples.
引文
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