Clinical Oral Investigations

, Volume 23, Issue 1, pp 33–41 | Cite as

Physical, chemical, and biological properties of white MTA with additions of AlF3

  • Marina Angélica MarcianoEmail author
  • Josette Camilleri
  • Ribamar Lazanha Lucateli
  • Reginaldo Mendonça Costa
  • Mariza Akemi Matsumoto
  • Marco Antonio Hungaro Duarte
Original Article



Addition of aluminum fluoride (AlF3) to MTA was tested to inhibit dental discoloration.

Materials and methods

MTA Angelus with 0, 5, 15, and 45% AlF3 were tested. The set cements were characterized using scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction. Radiopacity and setting time were analyzed according to ANSI/ADA 57 and ASTM C266-08. Volume change was evaluated using volumetric micro-CT analysis. The pH and calcium ion release were assessed after 3 and 24 h and 28 days. Dental discoloration in contact with the cements was assessed after 24 h and 28 and 90 days of contact with bovine and human dentine. Tissue reaction to subcutaneous implantation in rats was examined after 30 and 60 days.


AlF3 altered the microstructure of MTA. The addition of 5% AlF3 did not significantly alter the radiopacity, setting time, and volume change (p > 0.05). pH and calcium ion release significantly increased with addition of AlF3 (p > 0.05). All the tested proportions of AlF3 prevented the dental darkening verified for MTA Angelus in bovine and human teeth. AlF3 did not interfere in inflammatory response of MTA in all periods of analysis; otherwise, lower amounts showed less intense inflammatory infiltrate.

Clinical relevance

AlF3 prevents destabilization of bismuth oxide and consequent tooth darkening, frequently verified in clinical practice when using white MTA.


The use of 5% of AlF3 in combination to MTA resulted in a cement that did not result in dental discoloration and did not affect significantly physical, chemical, and biological properties.


Cement Biomaterials Biocompatibility Color 



The authors thank Ing. James Camilleri from the Department of Metallurgy and Materials Engineering of the University of Malta for his assistance. ERDF (Malta) for the financing of the testing equipment throughout the project: “Developing an Interdisciplinary Material Testing and Rapid Prototyping R&D Facility (Ref. no. 012).”


This work was supported by the State of São Paulo Research Foundation (FAPESP 2014/01003-6, 2017/05096-7).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Ethical approval

All applicable international, national, and/or institutional guidelines for the care and use of animals were followed.

Informed consent

For this type of study, formal consent is not required.


  1. 1.
    Farsi N, Alamoudi N, Balto K, Al Mushayt A (2006) Clinical assessment of mineral trioxide aggregate (MTA) as direct pulp capping in young permanent teeth. J Clin Pediatr Dent 31:72–76CrossRefGoogle Scholar
  2. 2.
    Bortoluzzi EA, Araujo GS, Guerreiro Tanomaru JM, Tanomaru-Filho M (2007) Marginal gingiva discoloration by gray MTA: a case report. J Endod 33:325–327. CrossRefGoogle Scholar
  3. 3.
    Akbari M, Rouhani A, Samiee S, Jafarzadeh H (2012) Effect of dentin bonding agent on the prevention of tooth discoloration produced by mineral trioxide aggregate. Int J Dent:563203.
  4. 4.
    Jacobovitz M, de Pontes Lima RK (2009) The use of calcium hydroxide and mineral trioxide aggregate on apexification of a replanted tooth: a case report. Dent Traumatol 25:e32–e36. CrossRefGoogle Scholar
  5. 5.
    Belobrov I, Parashos P (2011) Treatment of tooth discoloration after the use of white mineral trioxide aggregate. J Endod 37:1017–1020. CrossRefGoogle Scholar
  6. 6.
    Lenherr P, Allgayer N, Weiger R, Filippi A, Attin T, Krastl G (2012) Tooth discoloration induced by endodontic materials: a laboratory study. Int Endod J 45:942–949. CrossRefGoogle Scholar
  7. 7.
    Felman D, Parashos P (2013) Coronal tooth discoloration and white mineral trioxide aggregate. J Endod 39:484–487. CrossRefGoogle Scholar
  8. 8.
    Ioannidis K, Mistakidis I, Beltes P, Karagiannis V (2013) Spectrophotometric analysis of coronal discolouration induced by grey and white MTA. Int Endod J 46:137–144. CrossRefGoogle Scholar
  9. 9.
    Valles M, Mercade M, Duran-Sindreu F, Bourdelande JL, Roig M (2013) Influence of light and oxygen on the color stability of five calcium silicate-based materials. J Endod 39:525–528. CrossRefGoogle Scholar
  10. 10.
    Camilleri J (2008) Characterization of hydration products of mineral trioxide aggregate. Int Endod J 41:408–417. CrossRefGoogle Scholar
  11. 11.
    Camilleri J (2014) Color stability of white MTA in contact with hypochlorite solution. J Endod 40:436–440. CrossRefGoogle Scholar
  12. 12.
    Marciano MA, Costa RM, Camilleri J, Mondelli RFL, Guimarães BM, Duarte MAH (2014) Assessment of color stability of white MTA Angelus and bismuth oxide in contact with tooth structure. J Endod 40:1235–1240. CrossRefGoogle Scholar
  13. 13.
    Marciano MA, Camilleri J, Costa RM, Matsumoto MA, Guimarães BM, Duarte MAH (2017) Zinc oxide inhibits dental discoloration caused by white mineral trioxide aggregate Angelus. J Endod 43:1001–1007. CrossRefGoogle Scholar
  14. 14.
    Duarte MA, de Oliveira El KGD, Vivan RR, Guerreiro Tanomaru JM, Tanomaru Filho M, de Moraes IG (2009) Radiopacity of portland cement associated with different radiopacifying agents. J Endod 35:737–740. CrossRefGoogle Scholar
  15. 15.
    Camilleri J, Gandolfi MG (2010) Evaluation of the radiopacity of calcium silicate cements containing different radiopacifiers. Int Endod J 43:21–30. CrossRefGoogle Scholar
  16. 16.
    Marciano MA, Duarte MA, Camilleri J (2015) Dental discoloration caused by bismuth oxide in MTA in the presence of sodium hypochlorite. Clin Oral Investig 19:2201–2209. CrossRefGoogle Scholar
  17. 17.
    Marciano MA, Duarte MA, Camilleri J (2016) Calcium silicate-based sealers: assessment of physicochemical properties, porosity and hydration. Dent Mater 32:e30–e40. CrossRefGoogle Scholar
  18. 18.
    Cavenago BC, Pereira TC, Duarte MA, Ordinola-Zapata R, Marciano MA, Bramante CM, Bernardineli N (2014) Influence of powder-to-water ratio on radiopacity, setting time, pH, calcium ion release and a micro-CT volumetric solubility of white mineral trioxide aggregate. Int Endod J 47:120–126. CrossRefGoogle Scholar
  19. 19.
    Vosoughhosseini S, Lotfi M, Shahi S, Baloo H, Mesgariabbasi M, Saghiri MA, Zand V, Rahimi S, Ranjkesh B (2008) Influence of white versus gray mineral trioxide aggregate on inflammatory cells. J Endod 34:715–717. CrossRefGoogle Scholar
  20. 20.
    Asmussen E, Peutzfeldt A (2003) Strengthening effect of aluminum fluoride added to resin composites based on polyacid-containing polymer. Dent Mater 19:620–624. CrossRefGoogle Scholar
  21. 21.
    Williams JA, Briggs E, Billington RW, Pearson GJ (2003) The effects of adding fluoride compounds to a fluoride-free glass ionomer cement on subsequent fluoride and sodium release. Biomaterials 24:1301–1308. CrossRefGoogle Scholar
  22. 22.
    Bortoluzzi EZ, Broon NJ, Bramante CM, Felippe WT, Tanomaru-Filho M, Esberard RM (2009) The influence of calcium chloride on the setting time, solubility, disintegration, and pH of mineral trioxide aggregate and white Portland cement with a radiopacifier. J Endod 35:550–554. CrossRefGoogle Scholar
  23. 23.
    Wu MK, Wesselink PR, Boersma J (1995) A 1-year follow-up study on leakage of four root canal sealers at different thicknesses. Int Endod J 28:185–189. CrossRefGoogle Scholar
  24. 24.
    International Commission on Illumination. Recommendations on uniform colour spaces, colour difference equations, psychometric colour terms. CIE Publication No.15 (E-1.3.1) 1971/(TO-1.3) (Suppl. 15). Bureau Central de la CIE, Paris, France. 1978Google Scholar
  25. 25.
    Guimarães BM, Tartari T, Marciano MA, Vivan RR, Mondeli RFL, Camilleri J, Duarte MAH Color stability, radiopacity, and chemical characteristics of white mineral trioxide aggregate associated with 2 different vehicles in contact with blood. J Endod 41:947–952.
  26. 26.
    Parirokh M, Asgary S, Eghbal MJ, Kakoei S, Samiee M (2011) A comparative study of using a combination of calcium chloride and mineral trioxide aggregate as the pulp-capping agent on dog’s teeth. J Endod 37:786–788. CrossRefGoogle Scholar
  27. 27.
    Zmener O, Martinez Lalis R, Pameijer CH, Chaves C, Kokubu G, Grana D (2012) Reaction of rat subcutaneous connective tissue to a mineral trioxide aggregate-based and a zinc oxide and eugenol sealer. J Endod 38:1233–1238. CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Marina Angélica Marciano
    • 1
    Email author
  • Josette Camilleri
    • 2
  • Ribamar Lazanha Lucateli
    • 3
  • Reginaldo Mendonça Costa
    • 4
  • Mariza Akemi Matsumoto
    • 5
  • Marco Antonio Hungaro Duarte
    • 4
  1. 1.Department of Restorative Dentistry, Dental School of PiracicabaUniversity of Campinas - UNICAMPPiracicabaBrazil
  2. 2.School of DentistryUniversity of BirminghamBirminghamUnited Kingdom
  3. 3.Department of Surgery and Periodontology, Dental School of Ribeirão PretoUniversity of São Paulo – USPRibeirão PretoBrazil
  4. 4.Department of Dentistry, Endodontics and Dental Materials, Dental School of BauruUniversity of São Paulo – USPBauruBrazil
  5. 5.Department of Morphology, Dental School of AraçatubaState University of São Paulo – UNESPAraçatubaBrazil

Personalised recommendations