Interlab Comparison of Elemental Analysis for Low Ambient Urban PM 2.5 Levels (original) (raw)

Elemental analysis of airborne particulate matter by ED-XRF within the …

Ten residences in El Paso, TX were monitored in the summer of 2001 for concurrent indoor and outdoor PM 2.5 and PM 10 10-min mass concentrations in an attempt to establish the indoor-outdoor PM correlation for typical west Texas residences equipped with evaporative coolers. Simultaneously, the modified tapered element oscillating microbalance instruments were used to collect 48-h PM 2.5 and PM 10 samples, both indoor and outdoor, for elemental analysis. Water samples were also taken at each home for chemical and PM correlation analysis. The air and water samples were analyzed by inductively coupled plasma-mass spectrometry, with 30 elements identifiable above detection limits in the outdoor PM 10 samples and fewer elements in the PM 2.5 and indoor PM 10. Indoor elemental concentrations in PM 10 were found to be approximately 50-70% lower than outdoor concentrations in nine of ten homes, consistent with the PM 10 indoor/outdoor (I/O) mass concentrations previously reported. PM 2.5 I/ O ratio correlations were not as strong as for PM 10 ; however, reduced correlations could be attributed to a pattern of recurring outlier data pairs, consisting of the same three or four elements in all ten homes. Comparison of the elemental concentrations of the evaporative cooler supply water and indoor PM demonstrated little or no correlation, yielding a conclusion that the evaporative cooler was not introducing dissolved solids from the supply water into indoor air. Overall, evaporative cooling appears to provide a cleansing of indoor air.

Determination of trace elements in urban airborne particulates (PM10) using energy dispersive X-ray fluorescence (EDXRF) spectroscopy

Journal of Applied Sciences and Environmental Management, 2015

assessment of the air quality in Newcastle upon Tyne, UK was performed by determining the trace element content in airborne particulates (PM 10). Samples were collected over a 12 month period (March 2011 to April 2012) using two high volume air sampler provided with a PM 10 size selective inlet. The concentrations of 6 elements (Cr, Cu, Mn, Ni, Pb and Zn) were determined. The mean concentrations of these elements varied widely across the elements with Zn showing the highest concentration (41.3 ± 42.8 ng/m 3 ; ranging from 9.9-209.0 ng/m 3) and Cr the least concentration (1.7 ± 0.9 ng/m 3 ; ranging from 0.4-3.2 ng/m 3). The total elemental content obtained in this work was compared with regulatory limit values for 4 of the elements determined and it was discovered that none exceeded the limit values. © JASEM

Comparison of multiple X-ray fluorescence techniques for elemental analysis of particulate matter collected on air filters

Journal of Aerosol Science, 2018

This work reports on qualitative and semi-quantitative elemental analysis of particulate matter (PM) collected on PTFE membrane filters, for a source apportionment study conducted in Brescia (Italy). Sampling was undertaken in a residential area where an increase in Mn emissions has been highlighted by previous studies. Filters are measured by means of X-ray Fluorescence (XRF) based techniques such as micro-XRF and grazing incidence XRF using synchrotron radiation, Mo or W excitation sources, after applying an automatized sample preparation method. A heterogeneous distribution in PM shape, size and composition was observed, with features typical of anthropogenic sources. XRF measurements performed at various incidence angle, on large areas and different experimental setup were reproducible. The results demonstrate a successful comparison of the various XRF instrumentation, and the decrease in Mn content with the distance away from the identified emission source. This work highlights the potentialities of the presented approach to provide a full quantitative analysis, and ascertain its suitability for providing a direct, fast, simple and sensitive elemental analysis of filters in source apportionment studies and screening purposes.

Airborne particulate matter (PM) filter analysis and modeling by total reflection X-ray fluorescence (TXRF) and X-ray standing wave (XSW)

This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray standing wave (XSW) and total reflection X-ray fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample. Another advantage is related to the possibility to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XSW improve the accuracy of TXRF analysis.

Quality control materials for the determination of trace elements in airborne particulate matter

Analytical and Bioanalytical Chemistry, 2002

The development of quality control materials for the determination of selected trace elements in air pollution studies is described. Three types of test samples were prepared for proficiency testing: (1) filters loaded with PM10 fraction of urban air particulate matter (APM) using high-volume air samplers, which were subsequently divided into smaller sections, (2) a bulk sample of APM collected in an automobile tunnel in Prague, and (3) simulated air filters loaded with APM using a wet deposition process. Homogeneity of the test samples was studied using instrumental neutron activation analysis, proton induced X-ray emission and atomic absorption spectrometry, and inductively coupled plasma optical emission spectrometry and mass spectrometry. Sufficiently homogeneous samples were prepared by all three procedures. The simulated air filters appeared to be the most suitable test samples for proficiency testing.

Evaluation of standardless EDXRF analysis for the determination of elements on PM10 loaded filters

Atmospheric Environment, 2012

Energy Dispersive X-ray Fluorescence (EDXRF) was compared to Inductively Coupled Plasma Mass Spectrometer (ICP-MS) for the measurements of elements (Mg, Al, Si, S, Cl, K, Ca, Ti, V, Cr, Fe, Co, Ni, Mn, Cu, Zn, As, Br, Sr, Pb, Mo, Cd, Sn and Sb) in particulate matter (PM 10 ) collected on Teflon and two types of quartz filters at different sites. Two different methods of EDXRF analysis, linear calibration and standardless analysis, were studied. For the linear calibration, Pb, Mn, Fe, Cu, Ti and Zn were found to be site and filter type independent whereas Ca was only site independent. The site effect was evidenced for K, As, Ni, and V for quartz filter. The standardless EDXRF analysis showed better results than linear calibrations except for As, Co and V for Teflon filters and Cr and V for quartz filters. The measurement uncertainty of standardless EDXRF analysis was estimated by establishing a model equation. The measurement uncertainty estimated with this model equation was confirmed by field experiments provided that elemental masses exceeded observed thresholds. It was found that standardless EDXRF analysis is able to quantify most of the elements studied, particularly on Teflon filters rather than quartz filters. The standardless EDXRF analysis complies with the data quality objectives (DQO) of European Directives to measure Pb in PM 10 for three types of filters, even at concentrations lower than limit values (LV). The detection limits (MDL) of standardless EDXRF analysis for measuring As and Cd were found to be insufficient to meet the legislative requirements. The MDL of Ni was sufficiently low for measurements; however, measurement uncertainties remained higher than the DQO at the lower concentrations than LV.

Health-related monitoring and assessment of airborne particulate matter

Biological Trace Element Research, 1999

Since 1992, the International Atomic Energy Agency (IAEA) has been promoting studies of air pollution using a standard design of air sampler that provides separation on filters into two size fractions with cutoffs of 2.5 and 10 gm (approximately). These are the size ranges presently considered to have the most important health consequences. Such filter samples are highly amenable to analysis using nuclear and related techniques. After reviewing some of the health effects of airborne particulate matter and current air quality standards and guidelines, this article provides an overview of current and recent IAEA programs in this area, which involve collaborative activities with participants in more than 40 countries. Index Entries: Airborne particulate matter; PM10 and PM2.5; ambient air quality standards; Gent air sampler; nuclear analytical techniques; neutron activation analysis (NAA); particle-induced X-ray emission (PIXE); energy-dispersive X-ray fluorescence (ED-XRF); analytical quality control.

Determination of soluble ions and elements in ambient air suspended particulate matter: Inter-technique comparison of XRF, IC and ICP for sample-by-sample quality control

Talanta, 2009

In this paper, we describe a validation procedure for chemical fractionation analysis of elements (Al, As, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, S, Sb, Si, Sr, Ti and V) and soluble ions (Cl − , NO 3 − , SO 4 2− , Na + , NH 4 + , Mg 2+ , Ca 2+ ) in suspended particulate matter (PM). The procedure applies three distinct measurement techniques (XRF, IC and ICP-OES) to the analysis of individual samples. The techniques used generate different outputs at different stages in the procedure. This makes it possible to identify the contributions of specific parameters to measurement uncertainty. On this basis, we propose a scheme for controlling the analytical quality of data from individual samples in which inter-technique comparisons is used in the same way many analytical methods use surrogates. We apply this scheme to about 310 samples of PM 10 and PM 2.5 identifying and assessing the main factors contributing to measurement uncertainty. This procedure successfully resolved a number of difficulties frequently encountered during the analysis of PM, including lack of appropriate reference materials and the low reliability of alternative techniques of quality control. The results demonstrate the critical importance of sample treatment prior to destructive analysis by IC and ICP.