Quantitative Phase Analysis of Portland Cement Clinkers

X-ray powder diffraction combined with TOPAS Rietveld analysis is nowadays one of the most powerful methods existing, to perform quantitative phase analysis. In the last years it became a standard tool in cement industry for quality and process control, not only for clinker and cement analysis, but also for the whole process mineralogy.

TOPAS Rietveld phase quantification of the VDZ Round Robin Clinker sample (values given in wt. %). The blue curve is the measured diagram. The red curve is the calculated diagram. In grey the difference of both is given. The marks below indicate the possible peak positions of each phase.

Figure 1. TOPAS Rietveld phase quantification of the VDZ Round Robin Clinker sample (values given in wt. %). The blue curve is the measured diagram. The red curve is the calculated diagram. In grey the difference of both is given. The marks below indicate the possible peak positions of each phase.

A clinker sample of the 2005 VDZ Round Robin (German Cement Works Association) was analyzed, to demonstrate the performance of the D2 PHASER for such applications. The measurement covered the angular range from 10 to 65° 2Theta. The scan time was about 25 minutes. Figure 1 shows the measured data as well as the results of the TOPAS Rietveld analysis. Experimental details are summarized in Table 1.

Table 1. Experimental settings.

D2 PHASER, LYNXEYE detector
Cu radiation (30 kV, 10 mA), Ni filter
Continuous scan from 10 to 65° 2Theta,
Step width 0.02°
Counting time 0.5 sec per step
Total scan time about 25 min.
2.5° Soller slits, 1.0 mm divergence slit,
anti-scatter screen
LYNXEYE detector opening 5° 2Theta

Results VDZ Round Robin

The outcomes of the VDZ Round Robin are given in the table below.

Table 2. Outcomes of the VDZ Round Robin 2005. Mean values and standard deviation are given in wt.%.

Phase

mean esd

Alit(C3S)

71,55 2,63

Belit(C2S)

8,42 1,55

C3A kubisch

1,89 0,76

C3A orthorhombisch

5,32 1,08

Brownmillerit (C2(A,F))

9,39 1,05

Freikalk (Cao)

1,21 0,49

Periklas (Mgo)

0,71 0,22

Arcanit (K2SO4)

1,52 0,34

Summe C3Akub + C3Aorh

7,22 0,68

*in addition, we find Portlandite due to aging of the sample

The quantitative results compare well to the outcomes of the VDZ Round Robin (Table 2). There is an excellent agreement of ±1 wt.% for the main phases, with respect to the mean values of all participants.

Conclusion

To conclude, our cost-effective desktop XRD system D2 PHASER, equipped with the 1-dimensional LYNXEYE detector, provides high quality data, which allows doing reliable quantitative phase analysis of Portland Cement Clinkers and related applications

This information has been sourced, reviewed and adapted from materials provided by Bruker X-Ray Analysis.

For more information on this source, please visit Bruker X-Ray Analysis.

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