This datasheet demonstrates that the Epsilon 1, a benchtop energy dispersive X-ray fluorescence spectrometer, is more than capable of analyzing major, minor and trace elements in ceramic nanomaterials, in an easy and non-destructive way.
In the production of nanomaterials, catalysts are often used to enhance the formation of particles smaller than 100 nm. Nanomaterials are being used in many new applications. These include healthcare, composite materials, electrical and many other applications.
In the production of nanomaterials, catalysts are often used to enhance the formation of particles smaller than 100 nm. Nanomaterials are being used in many new applications.
These include healthcare, composite materials, electrical and many other applications. Catalyst residues can cause major and minor unwanted impurities in the nanomaterials which can affect their properties and therefore the final application. XRF analysis is a useful tool to monitor the impurities in the nanomaterials. This datasheet demonstrates that the Epsilon 1, a benchtop energy dispersive X-ray fluorescence spectrometer, is more than capable of analyzing major, minor and trace elements in ceramic nanomaterials, in an easy and non-destructive way.
Measurements were performed using an Epsilon 1 EDXRF spectrometer, equipped with a 50 kV silver-anode X-ray tube, 6 filters and high-resolution silicon drift detector. Automatic data processing was performed using the Epsilon 1 software.
Two commercially available ceramic nanomaterials (TiO2 and ZnO) were selected for analysis. The sample preparation was easy and fast. Small amounts (70-80 mg) of loose powder were put into a small-mass holder supported with a 6 µm polypropylene foil, and placed into the Epsilon 1 measuring station for analysis.
For characterization and analysis of ceramic nanomaterials where certified standards are not available, Malvern Panalytical’s Omnian standardless package is the solution of choice. The strengths of Omnian together with the ease of use of Epsilon 1 make it a powerful combination. As an out-of-the- box solution Omnian can be used to analyze a wide variety of elements in ceramic nanomaterials from sodium to americium across the periodic table. The total measurement time per sample was twenty minutes.
Figure 1. Seventy milligrams of a ceramic nanomaterial is placed into a disposable small-mass holder for analysis.
Figures 2 and 3 show XRF spectra of a TiO2 sample (80 mg), measured with different instrument conditions, while Figure 4 shows an XRF spectrum of a ZnO sample (70 mg).
Figure 2. XRF spectrum of a nano TiO2 sample obtained with Omnian showing unwanted impurities
Figure 3. The spectrum of a nano TiO2 sample obtained with Omnian showing unwanted impurities
Figure 4. The spectrum of a nano ZnO sample obtained with Omnian, showing unwanted impurities
The method repeatability was evaluated by making three freshly prepared samples of the same nanomaterial. For the TiO2 method repeatability test, each sample had a weight of 80 mg, while for the ZnO repeatability test each sample weighted 70 mg.
The average concentrations and RMS values (1 sigma standard deviation) for nano TiO2 samples from the method repeatability test are shown in Table 1.
Table 1. Repeatability results of 80 mg nano TiO2 , measured with Omnian
The results of the method repeatability test using nano ZnO samples is shown in Table 2. The average concentration and RMS values are shown. Even smaller amounts of material (e.g. 30 mg) can be quantified and the results are included in Table 2 for comparison. Being able to analyze smaller amounts of material is an advantage during the development of nanomaterials where the availability of material may be limited.
Table 2. Repeatability results of 70 mg of nano ZnO samples in comparison with even smaller amounts of 30 mg, measured with Omnian
Many minor and trace elements are present in the TiO2 and ZnO nanomaterials as impurities. The relatively low RMS values obtained from the TiO2 and ZnO repeatability tests show that sample preparation was reproducible and that Omnian in combination with Epsilon 1 is an easy and reliable analytical method.
The results clearly demonstrate the capability of Omnian standardless analysis software in combination with Epsilon 1 as an easy, economical and non-destructive analytical tool for quantifying compounds in ceramic nanomaterials. The high resolution and high sensitivity of the silicon drift detector combined with powerful software deconvolution algorithms make it possible to screen many major, minor and even trace elements in nanomaterials. Good results have been obtained for the method repeatability tests at small amounts of material of 70-80 mg.
