High Sensitivity Energy Dispersive X-Ray Fluorescence Spectrometer - Shimadzu EDX-7000/8000

The high-performance SDD detector and optimized hardware of the EDX-7000 and 8000 spectrometers from Shimadzu achieve an increased level of sensitivity, energy resolution and analysis speed that could not be attained previously. Detection from 6C is also possible with the EDX-8000 system.

The high-performance SDD detector and combined optimized optics and primary filters attain high sensitivity levels. Highly precise analysis is permitted in a short measurement time with the high fluorescent X-ray count per unit time (high count rate) of the SDD detector.

While studying samples generating a lot of fluorescent X-rays, such as samples with a metal as the main component element, this feature is achieved.

Key Features

The key features of the EDX-7000/8000 are:

  • The EDX-7000/8000 includes a high-count-rate SDD detector that achieves highly precise analysis of the target in a shorter measurement time when compared to the previous model. The EDX-7000/8000 instruments achieve very high energy resolution compared to previous models by including a sophisticated SDD detector. This minimizes the impact of overlapping peaks of different elements improving the consistency of analysis results.
  • The need for cooling by liquid nitrogen is eliminated as the SDD detector is electronically cooled. The user is hence freed from the chore of replenishing the liquid nitrogen and contributes to lower running costs.
  • An optional vacuum measurement unit or helium purge unit is required to measure light elements (15P and below) with the EDX-7000.
  • The EDX-8000 features an SDD detector with a special ultra-thin-film window material that is able to detect ultra-light elements such as carbon (C), oxygen (O), and fluorine (F)

Applications

  • Electrical/electronic materials
  • Automobiles and machinery
  • Ferrous/non-ferrous metals
  • Mining
  • Ceramics
  • Oil and petrochemicals
  • Chemicals
  • Environment
  • Pharmaceuticals
  • Agriculture and foods
  • Composition analysis of archeological samples and precious stones, analysis of toxic heavy metals in toys and everyday goods
  • The EDX-7000/8000 can accommodate samples up to a maximum size of W300 x D275 x approx. H100 mm.

Software

Shimadzu’s EDX-7000/8000 spectrometers are integrated with PCEDX Navi operating software that features a simple and refined user interface. The software provides easy instrument initialization and startup, intuitive operation and different report formats, making operators of all skill levels to easily use the system. The software can also handle more advanced research applications.

Simple Screen Layout

Sample image, selection of analysis conditions and sample name input are displayed on the same screen.

Collimator Switching from the Measurement Screen

The collimator diameter can be altered while observing the sample image while the selected diameter is represented by a yellow circle.

Automatic Storage of Sample Images

The sample image is automatically loaded after initiating the measurement procedure. The images are saved with a link to the data file.

Analysis of Inorganic Additives in Resin by FTIR and EDX

The quality of various products, such as food, plastic, electronic, cosmetic, and pharmaceutical products, can be improved by adding additives that improve the stability, workability, and functionality of the component materials in the product. These additives have a vital role in adding value to the products. The method used to analyze these additives depends upon whether the additive is organic or inorganic in nature. The first step in the analysis of organic additives involves the extraction of the additives, utilizing an appropriate pretreatment procedure. Then, an appropriate analytical instrument is employed to perform qualitative analysis after the chromatographic separation of the extracted components. Detailed identification of inorganic additives usually relies on the outcomes acquired using infrared spectroscopy, morphologic observation, elemental analysis, etc. Instances of FTIR analysis are demonstrated here, they are performed to acquire information related to certain typical inorganic additives. In addition, the application of the FTIR and the EDX to analyze an inorganic additive in a resin is also detailed.

Analysis of Inorganic Additives by FTIR

The principal application of FTIR is the analysis of organic additives. However, it can be also employed for the analysis of inorganic additives. A single-reflection ATR measurement was performed using a diamond prism in this example. The analytical conditions while using the FTIR are listed in Table 1.

Table 1. Analytical conditions using FTIR

Instruments : IR Tracer-100, Quest, Diamond
Resolution : 4.0 cm-1
Accumulation : 40
Apodization : Happ-Genzel
Detector : DLATGS

Figures 1 to 4 illustrate the peak positions and the infrared spectra of aluminum silicate, aluminum hydroxide, magnesium silicate, and calcium carbonate used as additives. The occurrence of a wide peak in the lower wavenumber region is a unique spectral characteristic of inorganic additives. As can be seen from Figures 1 to 3, at times, a typical peak occurs in the higher wavenumber region. Under such circumstances, only FTIR can be applied to make qualitative identification.

IR spectrum and peak position of Al2Si2O5(OH)4

Figure 1. IR spectrum and peak position of Al2Si2O5(OH)4

IR spectrum and peak position of Al(OH)3

Figure 2. IR spectrum and peak position of Al(OH)3

IR spectrum and peak position of Mg3Si4O10(OH)2

Figure 3. IR spectrum and peak position of Mg3Si4O10(OH)2

IR spectrum and peak position of CaCO3

Figure 4. IR spectrum and peak position of CaCO3

Analysis of Inorganic Additives in Resin

A connector cover containing an inorganic additive was analyzed using FTIR. A photograph of the sample is shown in Figure 5. The results of the analysis are illustrated in Figure 6.

Connector cover

Figure 5. Connector cover

IR spectra and FTIR search results for the analysis of the connector cover

Figure 6. IR spectra and FTIR search results for the analysis of the connector cover

Polyvinylchloride (PVC) was determined to be the main component of the connector cover, using the infrared spectra and FTIR search results illustrated in Figure 6. The presence of calcium carbonate (CaCO3) was indicated by a peak in the region of 1415 cm-1 in the infrared spectrum.

However, comparing the connector cover peak at 1415 cm-1 with the peak at 1390 cm-1 for CaCO3 alone demonstrated a shift of 25 cm-1 in the peak position. This means by only using the infrared spectrum, it cannot be undeniably concluded that calcium carbonate is included as the additive. To eliminate this variation, the analysis was conducted using the EDX technique. The analytical conditions while using the EDX are listed in Table 2. Figure 7 illustrates the qualitative analytical results. The results obtained from the EDX analysis are illustrated in Tables 3-1 and 3-2.

Table 2. Analytical conditions using EDX

   
Instrument : EDX-7000
X-ray tube : Rh target
Voltage/current : 15 kV(Na-Sc), 50 kV(Ti-U)/Auto
Atmosphere : Vacuum
Measurement diameter : 10 mmf
Integration time : 100 seconds

Results of qualitative analysis of the connector cover performed by using EDX

Figure 7. Results of qualitative analysis of the connector cover performed by using EDX

Table 3-1. Results A of quantitative analysis of the connector cover using EDX

Element Cl Ca Sb Zn Ti Si Al Cu Sr
Quantitation value (%) 72.56 26.11 0.40 0.31 0.23 0.21 0.096 0.054 0.030

Table 3-2. Results B of quantitative analysis of the connector cover using EDX

Element C2H3Cl CaCO3 SiO2 Sb2O3 TiO2 ZnO Al2O3 CuO SrO
Quantitation value (%) 73.14 25.55 0.31 0.30 0.25 0.25 0.13 0.046 0.024

As displayed in Table 3-1, calcium (Ca) and chlorine (Cl) are the main constituent elements. This result is in accordance with the polyvinylchloride results obtained using the FTIR, reiterating the presence of calcium carbonate. Table 3-2 illustrates the quantitative analytical results obtained for particular compounds determined from both FTIR and EDX results. The other elements detected are presumed to be oxides, so the FTIR and EDX combination has provided adequate evidence for the presence of calcium carbonate as an additive.

Conclusion

The combination of FTIR and EDX can be effectively used to make precise identification of the additives present in an actual sample. This type of analysis can be used for contaminant analysis as well as confirmation testing, and is recommended to perform confirmation testing of various products, such as electrical, electronic, chemical, food, pharmaceutical, cosmetic, and plastic products.

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