Design and evaluation of a new fully microwave-assisted liquid sample introduction device for inductively coupled plasma atomic emission spectrometry

Abstract

A new fully microwave-assisted liquid sample introduction system (MASIS) is presented and evaluated in Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The device employs a single TM₀₁₀ microwave cavity for the simultaneous aerosol generation and desolvation. The different experimental requirements of both physical processes demand a careful system design and a judicious selection of the experimental conditions. The behavior of the MASIS depends on the: (i) microwave power; (ii) nebulizer nozzle inner diameter; (iii) sample uptake rate; and, (iv) matrix nature (i.e. acids, salts) and concentration. Thus, optimum operating conditions are obtained when increasing the microwave power, the matrix concentration and the sample uptake rate as well as when decreasing the nebulizer nozzle inner diameter. The analytical figures of merit afforded by the MASIS in ICP-AES are compared to those obtained with: (1) a pneumatic concentric nebulizer coupled to a cyclonic spray chamber (CS); (2) a microwave thermal nebulizer (MWTN) coupled to a cyclonic spray chamber; and (3) a pneumatic nebulizer coupled to a microwave desolvation system (MWDS). MASIS provides limits of detection up to 50 times lower than those obtained with the CS and up to 8 times lower than those with the MWTN and MWDS. No significant difference in the signal precision between the different devices tested is observed (i.e. 2–5%). Regarding the wash-out times, both MASIS and MWDS show the highest values of this parameter (i.e. 70 s) due to their higher inner volume. Wash-out time values for both MWTN and CS are lower than 30 s.