Cement Analysis by Quantification XRD methods

Sietronics cement solution - Material, Software & Expertise

Material
The measurement of mineral phases in Portland Cement Clinker is very important in the Cement industry. The four main phases in clinker are Alite C3S, Belite C2S, Aluminate C3A, and ferrite C4AF. Minor amounts of periclase, arkanite, thenardite, anhydrite and other phases may also be present.

The advent of the Rietveld method and modern X-ray diffractometers (XRD) with high speed detectors has now made it practical to obtain the rapid, accurate and consistent phase analyses of clinker.
Benefits in quality and process control
Clinker
  • Rietveld analysis provides true clinker composition
  • Chemical and physical properties are mainly governed by the phase composition, not the elemental composition
  • Rietveld allows a rapid determination of phase contents in clinker and cement
 
Results
For the analysis, Siroquant has been used to quantify mineral phases in two NIST certified SRM’s, 2686 and 2687.
SIROQUANT was used to fit the full calculated XRD profile to the observed diffraction pattern by full-matrix least-squares refinement of the following parameters for each phase:
- SCALE FACTOR
- PREFERRED ORIENTATION
- UNIT CELL DIMENSION
- HALFWIDTHS (U, V, W)
- THE LINE SHAPE
Quantitative phase analysis from SIROQUANT shows close correlation with NIST certified values which fall
well within the quoted confidence limits. These analyses are detailed in the tables and scans below.
(Yellow Trace = Observed Diffraction Pattern from XRD)
(Red Trace = Full Calculated Profile from SIROQUANT)
(Blue Trace = Difference Pattern)
 
Software

SIROQUANT is a Rietveld based software developed by the CSIRO and Sietronics in Australia. One of the first commercial Rietveld packages on the market, it is used by hundreds of customers around the world. Siroquant is easy to use, requiring little to no crystallographic knowledge as crystal structure data is incorporated into the Crystal Structure Databank supplied with the software. This databank holds more than 1,700 common compounds, including the common cement phases found in Portland Cements. SIROQUANT has also been used to quantify cement hydration phases which are very important in the construction of more durable and stronger structures.
Siroquant features
In addition to quantification of the mineral phases using SIROQUANT, the crystallite size, chemistry via back calculation, cell parameters and amorphous content can also be determined. Batch processing allows users to easily perform quantification on large batches of samples, greatly reducing operator processing time. The included API also allows for automated processing of regular samples of similar expected composition. SIROQUANT has also been tested with many standard mixtures and has been used to quantify phases in: beach sands, Portland cement, fly ash, coal ash, opal, clays, sandstones, slags, bauxites, china clays, zeolites, zirconia ceramics, pharmaceuticals and more!
 
Experts
Sietronics is in this industry for more than 30 year, Our staff and consultants also have extensive experience in XRD 
Microscopy
• manual point counting
• direct method
• accurate for main phases
 
SEM image showing Halloysite, Gibbsite and Kaolinite
SEM image showing Halloysite Scrolls