Methodologies for measuring the setting times of mineral trioxide aggregate and Portland cement products used in dentistry

Abstract

Objective The current standard used to measure setting time for Mineral Trioxide Aggregate (MTA) involves indentation testing with arbitrary weights. This study compared indentation testing against rheological measurements and assessed the influences of particle size and the inclusion of bismuth oxide on the setting time of experimental MTA and Portland cement (PC).

Material and methods Two PCs (P1 and P2) of different particle sizes were produced using the same clinker. From these two PCs, two experimental MTAs (M1 and M2) were created with the addition of bismuth oxide. Particle size distributions were assessed using laser diffraction analysis. Indentation setting time tests were performed in accordance to the Gillmore needle test. Elastic modulus was assessed using a strain-controlled rheometer at 1 rad s⁻¹ and an applied strain of 0.01%.

Results P1, P2, M1 and M2 cements had median particle sizes of 6.1, 12.5, 6.5 and 13.0 μm, respectively. Using indentation testing, final setting times were ranked P1 < M1 < P2 < M2. The ranking of the final setting time corresponded with the rheological assessment of time required to reach 95% of the elastic modulus plateau.

Conclusions The time to reach 95% elastic modulus plateau of 9.3 min corresponds to a time close to the point where the material can be overlaid with another restorative material to give a final restoration. The 95% plateau value for elastic modulus may be a more useful parameter for determining how the setting reaction of PC and MTA cements progress over time.

Keywords:

• Mineral trioxide aggregate
• Portland cement
• particle size
• setting time
• rheology

Acknowledgements

The authors thank SiPowders Pty Ltd providing the cement powders in this study and Cement Australia Pty Ltd for assistance with laser diffraction testing. We thank Mingyuan Lu for assistance with indentation testing.

Declaration of interest

This study was supported by the Australian Dental Research Foundation (Grant 2011001653).