A new continuous calibration method for inductively coupled plasma spectrometry

摘要

A new calibration method was developed and applied to inductively coupled plasma atomic emission spectrometry. External calibration was performed as follows. A container was filled with a given volume of deionized (V-p) water. Then a concentrated standard was introduced at a controlled rate (Q(e)) into the tank by means of a peristaltic pump. The resulting solution was stirred throughout the experiment. Simultaneously, the solution inside the tank was pumped from the vessel to the plasma at a given rate (Q(s)). The signal was continuously recorded. The variation of the concentration of the solution leaving the tank with time was determined by applying a basic equation of stirred tanks. The representation of the emission intensity versus the time and the further conversion of the time scale into a concentration scale gave rise to the calibration line. The best results in terms of linearity were achieved for V-p = 15 cm(3), Q(e) = 0.6-0.75 ml min(-1) and Q(s) = 1-1.2 ml min(-1). Graphs with more than 40 standards were obtained within about 10 min. The results found were not statistically different from those afforded by the conventional calibration method. In addition, the new method was faster and supplied better linearity and precision than the conventional one. Another advantage of the stirred tank was that procedures such as dynamic calibration and standard additions could be easily and quickly applied, thus shortening the analysis time. A complete analysis following these procedures based on the measurement of 30 standards took about 5 min. Several synthetic as well as certified samples (i.e., bovine liver, mussel tissue and powdered milk) were analyzed with the stirred tank by applying four different calibration methodologies (i.e., external calibration, internal calibration, standard additions and a combination of internal standardization and standard additions), with the combination of internal standardization and standard additions being the method that provided the best results. The element concentrations obtained were not significantly different from the actual or certified values.