Water, Air, and Soil Pollution

, Volume 178, Issue 1, pp 323–334

Analysis of Environmental Samples Using Microwave-Assisted Acid Digestion and Inductively Coupled Plasma Mass Spectrometry: Maximizing Total Element Recoveries

  • Nouri M. Hassan
  • Pat E. Rasmussen
  • Ewa Dabek-Zlotorzynska
  • Valbona Celo
  • Heidi Chen
Article

DOI: 10.1007/s11270-006-9201-3

Cite this article as:
Hassan, N.M., Rasmussen, P.E., Dabek-Zlotorzynska, E. et al. Water Air Soil Pollut (2007) 178: 323. doi:10.1007/s11270-006-9201-3

Abstract

For the routine determination of metals in environmental samples, we require microwave-assisted digestion methods that yield ‘total’ or ‘near-total’ recoveries while avoiding the use of HF acid. As inductively coupled plasma mass spectrometry (ICP-MS) is the method of detection, it is desirable to minimize the use of HCl to avoid spectral interferences caused by high Cl concentrations. Using certified reference materials, we performed a series of modifications to the US EPA method 3051 which included: increasing the temperature and durations of microwave digestion, varying the ratio of sample mass to acid volume, and alterations to the compositions of the acid digestion mixture. The experiments were conducted using urban particulate matter (NIST-1648), coal fly ash (NBS-1633) and six CANMET certified reference materials (Till-2, Till-3, Till-4, LKSD-1, LKSD-2 and LKSD-4), in two laboratories (Health Canada and Environment Canada) using different microwave digestion systems and different ICP-MS instruments. Our modified microwave-assisted nitric acid digestion method improved recoveries for Pb, Zn, V, Fe and Cu approaching ‘total’ recoveries in the same matrices determined using X-ray fluorescence (XRF) and instrumental neutron activation analysis (INAA) as reported in the certificates of analysis. Recoveries for other elements such as Cr and Ni compared well with ‘near-total’ recoveries yielded by traditional (non-assisted) acid digestion methods.

Keywords

HNO3 ICP-MS microwave digestion sediments soil trace element analysis urban particulate matter 

Copyright information

© Springer Science + Business Media B.V. 2006

Authors and Affiliations

  • Nouri M. Hassan
    • 1
  • Pat E. Rasmussen
    • 1
  • Ewa Dabek-Zlotorzynska
    • 2
  • Valbona Celo
    • 2
  • Heidi Chen
    • 2
  1. 1.Safe Environments Program, HECS Branch, Health CanadaAL 0803C, OttawaCanada
  2. 2.Analysis and Air Quality DivisionEnvironmental Technology Centre, Environment CanadaOttawaCanada

Personalised recommendations