Online Standard Additions Calibration of Transient Signals for Inductively Coupled Plasma Mass Spectrometry

2007 ◽  
Vol 79 (2) ◽  
pp. 688-694 ◽  
Author(s):  
Margaret Antler ◽  
E. Jane Maxwell ◽  
David A. Duford ◽  
E. D. Salin
2000 ◽  
Vol 83 (2) ◽  
pp. 382-390 ◽  
Author(s):  
Eng-Shi Ong ◽  
Yuk-Lin Yong ◽  
Soo-On Woo

Abstract A simple, sensitive, and rapid method was developed for the determination of lead in botanicals and Chinese prepared medicines (CPM) by using closed-vessel microwave digestion with flow injection–inductively coupled plasma–mass spectrometry. The limits of detection and quantitation for the method, based on 0.5 g digested sample, were calculated to be 0.10 and 0.61 mg/kg, respectively. A simple approach was proposed for calibration by multiple linear regression (MLR) with 207Pb, 206Pb, and 204Pb for the determination of lead in botanical and CPM samples. The results from calibration by MLR were compared with those obtained by conventional modes using 207Pb and the sum of 207Pb and 206Pb. The results obtained by the different modes of calibration were in good agreement for botanical and CPM samples. The method was found to have good accuracy for the analysis of botanical reference materials. Method precision based on analyses of different types of CPM samples by different analysts on different days for different levels of lead was between 3.0 and 8.0% (relative standard deviation, n = 6). The effect of possible matrix interference caused by nitric acid and the extent of digestion was investigated with the method of standard additions. Significant matrix interference was not observed for the CPM samples analyzed. MLR was used to examine the effect of variation in isotopic abundance, which was found to present no significant problem in the determination of lead in the botanical and CPM samples.


2002 ◽  
Vol 56 (1) ◽  
pp. 62-69 ◽  
Author(s):  
Andrew M. Leach ◽  
Gary M. Hieftje

Low sample consumption and high achievable spatial resolution combine to make laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) an attractive direct sampling technique for the analysis of solids. These desirable characteristics are best realized when the laser ablation system is operated in a single-shot fashion, in which each laser pulse produces a transient analyte signal. The temporal width of a single-shot LA analyte transient is inversely related to the best achievable signal-to-noise ratio (S/N). Thus, production of fast transient signals is an important consideration in single-shot LA analyses. In this study we explore the effects on transient pulse width of ablation-cell volume, the diameter and length of tubing used to connect the ablation cell to the ICP, and the composition and flow rate of ablation-cell sweep gas. Minimization of ablation-cell volume and the length and diameter of the transfer tube was found to dramatically decrease the peak widths of transient signals. However, use of helium gas to sweep analyte particles from the ablation cell was found to significantly reduce the effect of cell volume on transient width. Use of a cell volume of 0.70 cm3 and optimization of other instrumental parameters produced a transient sample pulse 85 ms in duration and limits of detection in the tens of femtograms range for single-shot laser-ablation events.


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