Improvements in calibration procedures for the quantitative determination of trace elements in carbonate material...

A better repeatability and accuracy in the quantitative determination of trace elements in mussel shells or carbonate-based materials by LA-ICP-MS was achieved by using a series of multielement calibration standards prepared by co-precipitation of twelve elements into a CaCO3 matrix in order to improve the homogeneity of the resulting powder samples. Pressed powder discs of good mechanical stability could be obtained at a pressure of 50 MPa, without the addition of a binder. An UV laser (modified Nd:YAG, 266 nm) was used in the Q-switched mode at a repetition rate of 10 Hz and an energy level of 3.5 mJ. Correlation coefficients (R) for the linear calibration graphs (concentration range: 1.5-400 microg/g) for Cr, Mn, Co, Cu, Zn, As, Cd, Sn, Ba, and Pb are generally better than 0.997. The detection limits for all elements investigated are in the sub-microg/g range. Incorporation of elements into the matrix by co-precipitation has shown as a superior method for producing calibration standards than the simple mixture of the analytes (in carbonate or oxide form) with the matrix (CaCO3) or addition of standard solutions to a carbonate powder base. Two examples of the quantitative determination of toxic elements in mussel shells will be presented.