Development of an on-line low gas pressure cell for laser ablation-ICP-mass spectrometry

Anal Sci. 2007 Oct;23(10):1195-201. doi: 10.2116/analsci.23.1195.

Abstract

An on-line low gas pressure cell device has been developed for elemental analysis using laser ablation-ICP-mass spectrometry (LA-ICPMS). Ambient gas in the sample cell was evacuated by a constant-flow diaphragm pump, and the pressure of the sample cell was controlled by changing the flow rate of He-inlet gas. The degree of sample re-deposition around the ablation pit could be reduced when the pressure of the ambient gas was lower than 50 kPa. Produced sample aerosol was drawn and taken from the outlet of the diaphragm pump, and directly introduced into the ICP ion source. The flow rate of He gas controls not only the gas pressure in the sample cell, but also the transport efficiency of the sample particles from the cell to the ICP, and the gas flow rate must be optimized to maximize the signal intensity of the analytes. The flow rates of the He carrier and Ar makeup gas were tuned to maximize the signal intensity of the analytes, and in the case of (238)U from the NIST SRM610 glass material, the signal intensity could be maximized with gas flow rates of 0.4 L/min for He and 1.2 L/min for Ar. The resulting gas pressure in the cell was 30 - 35 kPa. Using the low gas pressure cell device, the stability in the signal intensities and the resulting precision in isotopic ratio measurements were evaluated. The signal intensity profile of (63)Cu obtained by laser ablation from a metallic sample (NIST SRM976) demonstrated that typical spikes in the transient signal, which can become a large source of analytical error, were no longer found. The resulting precision in the (65)Cu/(63)Cu ratio measurements was 2 - 3% (n = 10, 2SD), which was half of the level obtained by laser ablation under atmospheric pressure (6 - 10%). The newly developed low-pressure cell device provides easier optimization of the operational conditions, together with smaller degrees of sample re-deposition and better stability in the signal intensity, even from a metallic sample.