MICROCHEMICAL JOURNAL
·
2014
·
IF 3.583
Shengling Sun,Jie Li
A method has been developed for the determination of zirconium (Zr), hafnium (Hf), niobium (Nb), tantalum (Ta), molybdenum (Mo), tungsten (W), and tin (Sn) in seawater by quadrupole inductively coupled plasma-mass spectrometry (Q-ICP-MS). The method is based on separation of the seven elements by extraction chromatography using N-benzoyl-N-phenylhydroxylamine (BPHA) supported on a microporous acrylic ester polymeric resin. The optimized procedure indicates that the BPHA resin has high selective adsorption for Zr, Nb, Mo, Sn, Hf, Ta, and W (known as fluoride soluble elements), whereas other interference and matrix elements are minimally adsorbed. The optimized eluent mixture with their molarity gives satisfactory recoveries for all analytes. The recovery can be achieved 99% for Zr, 97% for Nb, 97% for Mo, 99% for Sn, 99% for Hf, 95% for Ta, and 98% for W, respectively, by eluting with 6 mL of 6 mol L − 1 HF/1 mol L − 1 HCl. Furthermore, the technique for separation and enrichment of these elements provides a low total method blank. The detection limits for this method are 0.5 ppt for Zr, 0.2 ppt for Nb, 1.7 ppt for Mo, 1.0 ppt for Sn, 0.1 ppt for Hf, 0.1 ppt for Ta, and 0.3 ppt for W, respectively. The validity of the method is evaluated by replicate analyses of seawater reference materials; the precision of the results is better than 3% (RSD, n = 4), and the results are in good agreement with certified values. The established procedure has proved to be both practical and effective for seawater sample analyses.
研究领域:
分析化学
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海洋化学
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环境地球化学
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痕量元素检测
·
质谱分析
✓ 已验证
DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2025
·
IF 3.4
Ai-qun Xiao,Pei-pei Zhao,Lu Yin,Bei Xu
A single-column extraction chromatographic purification method for tungsten using the N-benzoyl-N-phenylhydroxylamine (BPHA) resin was investigated in this study. This method greatly simplifies the W purification procedure, and only 10 ml of acid (5 ml 3 mol l -1 HCl-0.1 mol l -1 HF and 5 ml 1 mol l -1 HF) is required to separate W from Ti, Zr, Hf, Ta and other matrix elements. The blank in the separation step was less than 0.1 ng, and the recovery of W was ~ 99%. Six independent digestion measurements of reference materials BHVO-2, BCR-2, RGM-2 and JB-2 yielded μ 182 W values (mean value with intermediate precision, 95% confidence level) of -10.3 ± 4.0 ( n = 6, 2 s )，-1.2 ± 5.3 ( n = 6, 2 s )，-1.4 ± 4.4 ( n = 6, 2 s ) and 0.6 ± 3.8 ( n = 6, 2 s ), respectively, which are in good agreement with the previously reported values.
研究领域:
地球化学
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分析化学
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同位素地质学
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质谱分析
✓ 已验证
产品关联
DOI
高影响因子
Separations
·
2025
·Vol. 12
·期 8
·215
·
IF 2.7
Jiuquan Qi,Qianwen Chen,Chuanying Liu,Chengliang Xiao,Shuainan Ni
Due to the nearly identical chemical properties of Lu and Yb, the production of no-carrier-added (NCA)177Lu faces significant challenges in their separation. Achieving efficient and streamlined separation of Lu and Yb is crucial for the production of NCA177Lu. This study systematically investigated the separation performance of the commercial Rext-P350 extraction resin for Lu and Yb. Static adsorption experiments revealed that, at a solid–liquid ratio of 8 g/L, both Lu3+and Yb3+were nearly completely adsorbed, with saturation adsorption capacities of 25.8 mg/g and 21.5 mg/g, respectively. An increase in the nitric acid concentration in the aqueous phase significantly inhibited adsorption, but the separation factor for Lu3+/Yb3+remained above 1.88. The adsorption kinetics followed a pseudo-second-order model (R2> 0.99), with equilibrium reached within 15 min, demonstrating fast adsorption kinetics. Characterization by SEM, FT-IR, and XPS confirmed the chemical coordination between the resin and Lu3+/Yb3+. Dynamic chromatographic separation experiments showed that the Rext-P350 resin exhibited significantly better separation performance for Lu3+/Yb3+compared to 2-ethylhexylphosphoric acid mono-2-ethylhexyl ester (P507) extraction resin. Leveraging the excellent performance of Rext-P350 resin, a two-stage continuous extraction chromatography process was designed, achieving efficient separation of 0.045 mg of Lu3+from 200 mg of Yb3+with a Lu3+purity of 90.9% and a yield of 98.4%. This study provides a feasible separation technique for the purification of NCA177Lu.
研究领域:
核化学
·
放射性同位素生产
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分离科学
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无机化学
·
核医学
✓ 已验证
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2022
·
IF 8.008
Jieqing Feng,Qisheng Zhong,Ting Zhou
The online coupling technique of sample preparation with chromatography is a frontier topic in analytical chemistry since it minimizes errors caused by sample loss, shortens analysis time, and reduces solvent consumption. An online pressure change focusing-supercritical fluid selective extraction chromatography (PCF-SFSEC) technique was developed in this study, realizing extraction, purification, separation, and detection in a single run with only microliter-scale samples. The pressure change focusing strategy achieved column-head stacking by decreasing the dissolving capacity of the supercritical fluid, enabling the large volume introduction of extractants into supercritical fluid chromatography without causing peak broadening or distortion. All the extracts could be directly loaded into the chromatography system without split flow. Based on the supercritical fluid selective extraction (SFSE) strategy, the sorbents removed interferences and water from samples, effectively alleviating matrix effects and realizing the direct aqueous sample analysis. The efficiency of online PCF-SFSEC was demonstrated by the enantioselective analysis of 22 chiral drugs in rat plasma, covering eight categories with different pharmacological effects. The entire analysis took 25 min, consuming only 5 μL samples. All analytes in PCF-SFSEC obtained sharp and symmetrical peaks with resolutions higher than 1.0, and 86% had resolutions higher than 1.5. Limits of quantification (LOQs) ranged from 0.0600 to 32.1 μg/L. Recoveries were in the range of 75.8–117.2%. In addition, the developed approach obtained more satisfactory repeatability and significantly reduced matrix effects than conventional methods. The newly established online PCF-SFSEC technique is believed to be a green and powerful tool for the chiral analysis of complex samples.
研究领域:
分析化学
·
色谱技术
·
药物分析
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样品制备技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）