Spectrum stripping in rapid sequential atomic emission spectrometry with the inductively coupled plasma

摘要

Rapid sequential atomic emission spectrometry with the 'Zig Zag' acquisition system (ISA Jobin Yvon, France) in the case of the inductively coupled plasma is described. The 'Zig Zag' system is shown to enable the application of spectral stripping, as both the reproducibility of the intensities measured, for several lines of Fe, and the reproducibilty of the wavelength positioning (errors below 3 pm in the 2nd order and 5 pm in the lst order) were found to be high. Using an integration time of only 2.5 ms/point, the precision of the intensities expressed as the relative standard deviation is below 5%. These features are shown to allow spectrum stripping from the contribution of a Zr matrix, which has a rather line-rich atomic emission spectrum. Spectrum stripping was applied in the wavelength range from 237.9 to 241.1 nm, where 10 of the most sensitive emission lines of Fe were found. For sample solutions with 500 mg/l Zr only, 10 mg/l Fe only, 500 mg/l Zr as well as 10 mg/l Fe, and for a blank solution, respectively, five spectral scans were averaged and the averaged spectral scan for a blank solution was subtracted. The spectral scan obtained for a solution containing 500 mg/l Zr only was subtracted from the one obtained for the solution containing both 500 mg/l Zr and 10 mg/l Fe. The result of spectral stripping is comparable to the experimentally obtained spectral scan for the solution containing 10 mg/l Fe only after blank subtraction. The recovery for Fe was found to be 93 +- 2% and is therefore comparable to the one obtained by chemical separation methods using solvent extraction. When using an integration time of 50 ms per measurement point instead of 0.5 ms/point, as it is possible in the case of the 'Zig Zag' approach, the detection limit for Fe in the measurement solutions can be improved from 20 down to 3 #mu#g/1, or from 40 to 6 #mu#g/g Zr, respectively.