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Previous studies using scanning electron microscopy and infrared absorption spectroscopy reported that laser irradiation causes compositional changes in enamel. The purpose of this study was to evaluate the ultrastructural and compositional changes in dentin caused by irradiation with a short-pulse laser (Q-switched Nd:YAG). The irradiated and non-irradiated areas of the lased dentin samples were investigated by scanning (SEM) and transmission electron microscopy (TEM), micro-micro electron diffraction, and electron microprobe analysis of dispersive energy (EDX). Heat-treated dentin was similarly investigated. This study demonstrated that laser irradiation resulted in the recrystallization of dentin apatite and in the formation of additional calcium phosphate phases consisting of magnesium-substituted beta-tricalcium phosphate, beta-TCMP, beta-(Ca,Mg)3(PO4)2, and tetracalcium phosphate, TetCP, Ca4(PO4)O. TEM analyses of the modified and unmodified zones of the irradiated areas showed two types of crystal populations: much larger crystals from the modified zone and crystals with size and morphology similar to those of dentin apatite in the unmodified zone. The morphology of crystals in the modified zones in the irradiated dentin resembled those of dentin sintered at 800 or 950 degrees C. In the irradiated areas (modified and unmodified zones), the Ca/P ratio was lower compared with that in the non-irradiated dentin. The Mg/Ca ratio in the modified zones was higher than that in the unmodified zones and in the non-irradiated dentin. In sintered dentin, the Mg/Ca ratio increased as a function of sintering temperature. The ultrastructural and compositional changes observed in laser-irradiated dentin may be attributed to high temperature and high pressure induced by microplasma during laser irradiation. These changes may alter the solubility of the irradiated dentin, making it less susceptible to acid dissolution or to the caries process.

The use of x-ray photoelectron spectroscopy for the study of biological materials has provided mixed results. The experimental difficulties associated with the application of this technique to the study of biological materials include the effects of ultra-high vacuum, x-ray exposure, surface charging, and, for insulating materials, the inherent lack of an intrinsic energy reference. Since most biological materials are insulators, the lack of an intrinsic energy reference complicates one's ability to draw direct comparisons between different studies. In this paper, the results from two different apatites are compared with the results obtained from the use of two conventional techniques for referencing binding energies. The results presented here are referenced only to the Pt Fermi level; no further energy modifications are performed. A comparison with the results of other investigators indicates a large difference in binding energies for all involved core levels. These results indicate that, in the study of insulating materials with x-ray photoelectron spectroscopy, it is essential that all data be acquired under exacting conditions on the same experimental system.

The chemical and crystallographic events associated with the caries process can be described based on the results from the following studies: (a) effects of carbonate, magnesium, fluoride, and strontium on the physico-chemical properties--lattice parameters, crystallinity (crystal size and strain); dissolution properties of synthetic apatites; (b) factors influencing the in vitro formation and transformation of DCPD, OCP, AP (Ca-deficient apatites), FAP, beta-TCMP (Mg-substituted), and CaF2; and (c) studies on properties (crystallinity, composition, chemical, and thermal stabilities) of enamel, dentin, and bone. The dissolution of CO3-rich/Mg-rich/F-poor dental apatite crystals and re-precipitation of CO3-poor/Mg-poor/F-rich apatite in the presence of F- ions in solution contribute to a more acid-resistant surface layer of the caries lesion. Fluoride promotes the formation of less Ca-deficient and more stable apatite crystals. The presence of Ca, P, and F in solution inhibits dissolution of apatite more than does the presence of F alone. Low levels of F in solution promote the formation of (F, OH)-apatite, even under very acid conditions; an increase in F levels causes the formation of CaF2 at the expense of DCPD or apatite, especially in acid conditions. F in apatite and/or in solution suppresses extensive dissolution of dental apatite and enhances the formation of (F, OH)-apatite crystals which are more resistant against acid-dissolution than are F-free apatite crystals.

In vitro caries-like lesion formation in F-containing tooth enamel (shark) showed a lower depth of penetration compared to that in human enamel (42 vs. 100%). After longer periods of exposure, the depth of penetration in shark enamel is only 33% relative to that in human enamel. The extent of dissolution in acetate buffer for powdered human enamel and for synthetic F-free calcium-carbonated-apatites was greater than for powdered shark enamel and for synthetic F-containing apatites. These results suggest that the cariostatic action of fluoride may be explained in terms of a combination of two effects: (a) the stabilizing effect against acid dissolution (caries) when fluoride is incorporated in the tooth mineral (apatite), and (b) a greater degree of remineralization (repair) in the presence of F solution.

Physico-chemical investigations of enamel from deciduous teeth of a small number of children with and without pre-natal fluoride supplementation (PNF) exhibited the following differences between the PNF and non-PNF enamel, with the former showing: (a) more homogeneous and less extensive patterns of acid-etching; (b) denser crystal populations in intra-prismatic regions; (c) larger prism dimensions; (d) greater total mineral density (wt%ash); (e) higher degree of crystallinity; (f) smaller a-axis dimensions; and (g) more fluoride and less carbonate contents. On the basis of these preliminary findings, further studies with larger numbers of samples would seem appropriate.

Dental calculus from the dog was found to consist principally of the calcite form of calcium carbonate mixed with small amounts of apatite; other calcium phosphates, consistently present in human calculus, were not present in dog calculus. Precipitable calcium salts from human saliva were mainly apatite; for the dog the principal precipitated salt was calcium carbonate (calcite form).

This study correlated ultrastructural observations on the presence of beta-tricalcium phosphate (beta-TCP) in arrested dentin caries with physico-chemical observations on the in vitro formation of Mg-substituted beta-TCP. The ultrastructural studies were made using high-resolution transmission electron microscopy (TEM) with the capability of microdiffraction and microanalysis on sites less than 10 nm in diameter. Mg-substituted beta-TCP was obtained, by a precipitation method, from solutions with Mg/Ca molar ratios of 5/95 and higher. Such correlations led to the postulation of a possible chronological sequence of physico-chemical events occurring at the crystal level during the progress and arrest of caries in human dentin. It is suggested that the initial mechanism for the observed occurrence of large crystals of Mg-substituted beta-TCP and of apatite in the tubule lumen is due to the dissolution of the dentin mineral (a CO3- and Mg-rich calcium OH-apatite) and reprecipitation of Mg-substituted beta-TCP, followed by that of CO3- and Mg-poor apatite.