Total X-ray Fluorescence Spectroscopy (TXRF) Contact: World Agroforestry Centre (ICRAF), P.O. Box...
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Transcript of Total X-ray Fluorescence Spectroscopy (TXRF) Contact: World Agroforestry Centre (ICRAF), P.O. Box...
Total X-ray Fluorescence Spectroscopy (TXRF)
Contact: World Agroforestry Centre (ICRAF), P.O. Box 30677-00100 Nairobi, Kenya. Tel: +254 020 722 4000. www.worldagroforestry.org
•TXRF is a versatile analytical technique for determining
elemental content in liquids, solids and loose powders.
•The main principle is that atoms, when irradiated with X-rays,
radiate secondary X-rays – the fluorescence radiation.
•Each element is associated with a specific wavelength and
energy of the fluorescence radiation.
•The concentration of each element is calculated using the
fluorescence intensity.
•TXRF combines high accuracy and precision with simple and
fast sample preparation for the analysis of elements from
Sodium (Na; 11) to Uranium (U; 92) in concentration ranges
from 100% to sub-ppm level.
•TXRF is a powerful diagnostic tool for agriculture and
environment.
•TXRF analysis is suitable for all types of samples
• Sample digestion is not normally required.
•Samples are prepared on a sample tray
that reflects X-ray radiation.
• Trays have a diameter of 30 mm,
made of acrylic or quartz glass.
•Liquids are prepared directly on the sample tray.
• Several μl are transferred to the glass disc
using a pipette and evaporated (Figure 2).
•Powdered samples are finely ground (<50 μm),
prepared in suspensions and transferred to the
sample tray.
•Powder samples (a few μg of sample) can also
be transferred directly, using a Q-tip,
for semi-quantitative analysis.
IntroductionIntroduction
•Typical Lower Limits of Detection (LLD) are presented in
Figure 5.
•The LLD for many elements is 1-10 μg/l.
•Elements from Na (11) to U (92) are detected
•Applications include:
•Plant trace element diagnostics
•Soil element fingerprinting
•Soil heavy metal screening
•Soil solution/extract analysis
•Water quality analysis
Detection limits - ApplicationsDetection limits - Applications
•All elements from Sodium to Uranium (excl. Niobium,
Molybdenum and Technetium) can be analyzed (Figure 1).
•TXRF analysis is based on
internal standardization;
an element, which is not
present in the sample, must
be added for quantification
purposes (Figure 4).
•Measurement of the
complete spectrum;
all detectable elements
are measured
simultaneously.
Analysis and QuantificationAnalysis and Quantification
Sample types and preparationSample types and preparation
• The working principle of TXRF spectroscopy as realized in the
S2 PICOFOX spectrometer is shown in Figure 3.
• A primary beam generated by a X-ray tube is
monochromatized by Bragg-reflection on a Ni/C multilayer.
• Monochromatized X-rays hit a polished sample carrier (quartz
glass or acrylic glass) at a very shallow angle of incidence.
• X-rays are totally reflected by the surface of the sample
carrier at a very small angle (0.3 – 0.6 °).
• Fluorescence radiation is emitted only by the sample
deposited on the carrier surface.
• The characteristic fluorescence radiation emitted by the
sample is detected by an energy-dispersive detector.
• Intensity is measured by means of an amplifier coupled to a
multichannel analyzer.
TXRF Working PrincipleTXRF Working Principle
Fig. 1: Elements analyzed; Na (11) to U (92)
Fig. 4: Typical spectrum showing peaks of several elements
Fig. 3: Schematic working principle of the S2 PICOFOX spectrometer
Fig.2: Sample preparation steps for the TXRF analysis of liquids
S2 PICOFOX TXRF spectrometer
Fig. 5. Lower Limits of Detection
•Fast and simple sample preparation; no need for pressed
pellets
•Simultaneous multi-element trace analysis without external
calibration
•Analysis of small sample amounts in nanogram or microgram
range
•Suitable for various sample types: solids, powders, liquids,
suspensions
•Portable system for fast in-field analyses; low power rating
•Low maintenance and operating cost
•Highly reproducible
•Low limits of detection
Key advantages of TXRFKey advantages of TXRF
Sample trays