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|Title:||Method development for the determination of alkali metals in samples from pyrochemical reprocessing using ICP-OES and comparison with sector field ICP-MS.|
|Authors:||KRACHLER MICHAEL; VAN WINCKEL Stefaan; CARDINALE Mariangela; LYNCH Brian; MURAKAMI Tsuyoshi|
|Citation:||MICROCHEMICAL JOURNAL vol. 105 p. 9-14|
|Publisher:||ELSEVIER SCIENCE BV|
|Type:||Articles in periodicals and books|
|Abstract:||An analytical procedure for the reliable determination of the alkaline elements Na, K, and Li in radioactive samples was developed and validated. To this end, a high efficiency, desolvating nebulizer was coupled to a commercial high resolution ICP-OES instrument. Because of their radioactive nature, all investigated samples were handled in appropriate glove boxes operated in under-pressure, following strict safety and security procedures. After optimization of the ICP-OES operational parameters, detection limits (LODs) of 0.15 µg/L, 0.8 µg/L, and 1.3 µg/L were obtained for Li (=670.784 nm), Na (=589.592 nm), and K (=766.490 nm). Compared to conventional sample uptake rates of 1-2 mL/min, the 350 µL/min used in this study helped to lower the radiation dose to the ICP-OES operator and produced much less radioactive waste while at the same time improving LODs. Calibration curves were linear up to 4 mg/L with a correlation coefficient of better than 0.999. Because of its robust and reproducible performance, no internal standard was required to correct for potential drifts in sensitivity of the ICP-OES. Three certified water reference materials (BCR®-617, LGC6177, SRM® 1643a) were employed to assess the accuracy of the developed ICP-OES procedure, the results of which underpin its reliability. In addition, Na and K concentrations calculated from emission intensities measured at two wavelengths confirmed that each dataset is consistent in itself. A comparison of sector field ICP-MS results of 23 samples originating from pyrochemical reprocessing with the data obtained applying the newly developed ICP-OES procedure revealed that the latter provides a reliable, straightforward and more robust analytical approach to analyze Na, K, and Li in radioactive specimens. Keywords: ICP-OES, ICP-MS, Lithium, Sodium, Potassium, Comparison|
|JRC Directorate:||Nuclear Safety and Security|
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