Analysis of Antarctic marine sediment by inductively coupled plasma atomic emission and total reflection X-ray fluorescence spectrometry

Microwave digestion and extraction techniques were developed for elemental analysis of Antarctic marine sediment by inductively coupled plasma atomic emission spectrometry (ICP-AES) and total reflection X-ray fluorescence (TXRF) spectrometry. These sample preparation techniques were tested by analyzing river sediment certified reference material (BCR-320). Con centrations of Al, Fe, Mn, Zn, Cr, Co, and Cu were determined by ICP-AES after microwave digestion of sediment in a mixture of HF + HNO3 + HCl + H3BO3 with acceptable accuracy. Due to the strong matrix effect and spectral interference, Cd, Sn, Pb, Ni, and As cannot be determined using ICP-AES; however, the proposed microwave extraction procedure appears to be suitable for measurement of Zn, Cu, Pb, Ni, and As using TXRF spectrometry. (C) 1997 Academic Press.