Preparation of lead (Pb) X-ray fluorescence reference materials for the EPA Pb monitoring program and the IMPROVE network using an aerosol deposition method

Abstract

X-ray fluorescence (XRF) is a commonly used analytical method to quantify lead (Pb), a toxic element, in atmospheric aerosol. The commercially available reference materials used for calibrating XRF do not mimic the concentrations and filter materials of particulate matter (PM) monitoring networks. In this study, we described an aerosol deposition method to generate Pb reference materials (RMs) over a range of concentrations to serve several purposes for the US Environmental Protection Agency (EPA) and Interagency Monitoring of PROtected Visual Environments (IMPROVE) monitoring networks including laboratory auditing, federal equivalency method evaluation, and calibration and quality control of XRF instruments. The RMs were generated using a laboratory-built aerosol chamber equipped with a federal reference sampler at concentration levels ranging from 0.0125 to 0.70 g/m3. XRF analysis at UC Davis was demonstrated to be equivalent to a US and EU reference method, inductively coupled plasma - mass spectrometry (ICP-MS), for measuring Pb on RMs following a methodology described in the United States and international standards. The Pb concentrations on subsets of the RMs were verified by three other XRF laboratories with different analyzers and/or quantification methods and were shown to be equivalent to the UC Davis XRF analysis. The generated RMs were demonstrated to have short and long-term stability, satisfying an additional requirement of reference materials.