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Selective Micellar Extraction of Ultratrace Levels of Uranium in Aqueous Samples by Task Specific Ionic Liquid Followed by Its Detection Employing Total Reflection X-ray Fluorescence Spectrometry
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-09-14 00:00:00 , DOI: 10.1021/acs.analchem.7b02427 Abhijit Saha 1 , Kaushik Sanyal 1 , Neetika Rawat , Sadhan Bijoy Deb , Manoj Kumar Saxena , Bhupendra Singh Tomar
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-09-14 00:00:00 , DOI: 10.1021/acs.analchem.7b02427 Abhijit Saha 1 , Kaushik Sanyal 1 , Neetika Rawat , Sadhan Bijoy Deb , Manoj Kumar Saxena , Bhupendra Singh Tomar
Affiliation
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A task specific ionic liquid (TSIL) bearing phosphoramidate group, viz., N-propyl(diphenylphosphoramidate)trimethylammonium bis(trifluoromethanesulfonyl)imide, was synthesized and characterized by 1H NMR, 13C NMR, 31P NMR, and IR spectroscopies, elemental (C H N S) analysis, and electrospray ionization mass spectrometry (ESI-MS). Using this TSIL a cloud point extraction (CPE) or micelle mediated extraction procedure was developed for preconcentration of uranium (U) in environmental aqueous samples. Total reflection X-ray fluorescence spectrometry was utilized to determine the concentration of U in the preconcentrated samples. In order to understand the mechanism of the CPE procedure, complexation study of the TSIL with U was carried out by isothermal calorimetric titration, liquid–liquid extraction, 31P NMR and IR spectroscopies, and ESI-MS. The developed analytical technique resulted in quantitative extraction efficiency of 99.0 ± 0.5% and a preconcentration factor of 99 for U. The linear dynamic range and method detection limit of the procedure were found to be 0.1–1000 ng mL–1 and 0.02 ng mL–1, respectively. The CPE procedure was found to tolerate a higher concentration of commonly available interfering cations and anions, especially the lanthanides. The developed analytical method was validated by determining the concentration of U in a certified reference material, viz., NIST SRM 1640a natural water, which was found to be in good agreement at a 95% confidence limit with the certified value. The method was successfully applied to the U determination in three natural water samples with ≤4% relative standard deviation (1σ).
中文翻译：
特定任务离子液体选择性胶束萃取水溶液中痕量铀的超痕量铀，然后采用全反射X射线荧光光谱法对其进行检测
合成了具有氨基磷酸酯基团的任务特定离子液体（TSIL），即N-丙基（二苯基磷酸氨基酯）三甲基铵双（三氟甲磺酰基）酰亚胺，并通过1 H NMR，13 C NMR，31进行了表征P NMR和IR光谱，元素（CHNS）分析和电喷雾电离质谱（ESI-MS）。使用该TSIL，开发了浊点萃取（CPE）或胶束介导的萃取程序，用于对环境水性样品中的铀（U）进行预浓缩。利用全反射X射线荧光光谱法测定预浓缩样品中U的浓度。为了了解CPE程序的机理，通过等温量热滴定，液-液萃取法对TSIL与U进行络合研究311 H NMR和IR光谱，以及ESI-MS。先进的分析技术对铀的定量萃取效率为99.0±0.5％，预浓系数为99。该方法的线性动态范围和方法检测极限为0.1–1000 ng mL –1和0.02 ng mL – 1个， 分别。发现CPE程序可耐受较高浓度的常用干扰阳离子和阴离子，尤其是镧系元素。通过确定经认证的参考物质（即NIST SRM 1640a天然水中）中U的浓度，验证了开发的分析方法，该标准物质与认证值在95％的置信度范围内吻合良好。该方法已成功用于相对标准偏差≤4％的三个天然水样中U的测定。
更新日期：2017-09-15
中文翻译：
特定任务离子液体选择性胶束萃取水溶液中痕量铀的超痕量铀，然后采用全反射X射线荧光光谱法对其进行检测
合成了具有氨基磷酸酯基团的任务特定离子液体（TSIL），即N-丙基（二苯基磷酸氨基酯）三甲基铵双（三氟甲磺酰基）酰亚胺，并通过1 H NMR，13 C NMR，31进行了表征P NMR和IR光谱，元素（CHNS）分析和电喷雾电离质谱（ESI-MS）。使用该TSIL，开发了浊点萃取（CPE）或胶束介导的萃取程序，用于对环境水性样品中的铀（U）进行预浓缩。利用全反射X射线荧光光谱法测定预浓缩样品中U的浓度。为了了解CPE程序的机理，通过等温量热滴定，液-液萃取法对TSIL与U进行络合研究311 H NMR和IR光谱，以及ESI-MS。先进的分析技术对铀的定量萃取效率为99.0±0.5％，预浓系数为99。该方法的线性动态范围和方法检测极限为0.1–1000 ng mL –1和0.02 ng mL – 1个， 分别。发现CPE程序可耐受较高浓度的常用干扰阳离子和阴离子，尤其是镧系元素。通过确定经认证的参考物质（即NIST SRM 1640a天然水中）中U的浓度，验证了开发的分析方法，该标准物质与认证值在95％的置信度范围内吻合良好。该方法已成功用于相对标准偏差≤4％的三个天然水样中U的测定。
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