Wednesday, December 27, 2006

Analysis of Environmental Contamination by Heavy Metals and Metalloids by X-Ray Fluorescence Using the MiniPal 2 from PANalytical

Background

Environmental contamination by heavy metals and metalloids (particularly Arsenic) have occurred at former sites of industrial and agricultural activity. The extent of contamination of surface and ground waters needs to be known before site remediation can take place.

In waters, the concentration of such analytes is often below detection. Evaporation of water onto a surface such as x-ray film constitutes a pre-concentration phase allowing the effective lowering of detection limits for dissolved analytes.
Instrumentation

A PANalytical MiniPal 2 equipped with a 30 kV Rhodium anode tube, 5 different filters and a high-resolution solid state detector was used.

Although a Helium purge is available for light element sensitivity enhancement this was not necessary in this case for the heavier elements analysed here.
Procedure

Synthetic standard solutions were mixed in various ratios and 500 μL of the resulting solution was pipetted onto a dimpled ProleneTM target. The targets were dried under a 100 W light bulb for 12 hours and loaded into the spectrometer. Two excitation conditions were used to acquire the spectra (Table 1). Matrix correction was made by ratioing to a background channel, Bg, with a Region Of Interest (ROI) of 15.300 to 16.000 keV.

Table 1. All elements were measured using their Kα line except Ag, Cd, Sn, and U which were measured using their Lα1 lines and Pb where the Lβ1 line was used.

Element

kV

µA

Filter

Medium

Counting Time
(sec)

As,Bg,Cu,Pb,U,Zn

30

300

Mo

Air

100

Ag,Al,Cd,Cr,Fe,Ni,Sn

15

40

Al_thin

Air

100