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Differences in intensity/resolution due to differences in X-ray tubes

Background

With the MiniFlex, it is possible to select a fine focus tube (focal point size 0.4 x 8 mm²) in addition to a normal focus tube (focal point size 1 x 10 mm²) of the type generally used with powder X-ray diffractometers.

Investigation

Fig. 1 shows an overlay of diffraction peaks obtained by measuring with a normal focus tube and fine focus tube. Table 1 shows a comparison of intensity, and full width at half maximum (FWHM), which varies proportionally with resolution.

 Intensity ratios and full width at half maximum due to differences in focal point size
Table 1: Intensity ratios and full width at half maximum due to differences in focal point size

 

Fig. 1:Comparison of normal focus tube and fine focus tube
Figure 1: Comparison of normal focus tube and fine focus tube

 

 

Both intensity and resolution can be improved by using a fine focus tube. Therefore, these tubes are suitable for measuring samples with many peaks, and samples containing trace components. Fig. 2 shows qualitative analysis results, and quantitative analysis results using the Rietveld method, for a cement sample (NIST 2686 standard material). In the analysis results, there was a good match, within the error range, between the content of each crystal phase, and the standard values for NIST 2686 standard material.

Qualitative and quantitative analysis results for cement sample
Figure 2: Qualitative and quantitative analysis results for cement sample (NIST 2686 standard material)

 

Apparatus conditions:

MiniFlex600 (F.F tube), Detector: D/teX Ultra, Slit conditions: DS = 0.625°, SS = 8 mm, RS = open, Incident side and receiving side Soller slit: 5°, Incident height limiting slit = 10 mm

Measurement conditions:

Scan range: 2θ = 5 ~ 90°, Step width: 0.02°, Scan speed: 5° / min. (about 18 min.)