Interfacial chemistry of the dentin/adhesive bond.

To date, the dentin/adhesive (d/a) bond has primarily been studied by morphologic analysis in conjunction with bond strength measurement. Although these analyses have enhanced our understanding, numerous questions about the chemistry have not been answered. The purpose of this study was to determine, at the molecular level, quantitative differences in the composition of the d/a interface formed under "wet" bonding conditions. The occlusal one-third of the crown was removed from 10 extracted, unerupted human third molars. The prepared dentin surfaces were treated, per manufacturers' instructions, with either Single Bond (3M) or One-Step adhesive (Bisco). Three-micron-thick sections of the d/a interface were cut and stained with Goldner trichrome for light microscopy. Companion slabs were analyzed with micro-Raman spectroscopy; the sample was placed at the focus of a 100x microscope objective, and spectra were acquired at 1-microm intervals across the d/a interface. Reference spectra were collected on model compounds of type I collagen and adhesive; the relative ratios of the integrated intensities of spectral features from adhesive and collagen were determined and plotted as a function of wt% adhesive. The same ratios were determined for the interface samples; by comparing these ratios with the calibration curve generated from the model compounds, we determined the percent of adhesive as a function of spatial position across the d/a interface. The relative percent of Single Bond adhesive was < 50% throughout more than half of the hybrid layer; One Step adhesive was > or = 50% throughout most of the hybrid. The results from this study provide the first direct chemical evidence of phase separation in a dentin adhesive and its detrimental effect on the dentin/adhesive bond.

Spectroscopic and morphologic characterization of the dentin/ adhesive interface.

The potential environmental risks associated with mercury release have forced many European countries to ban the use of dental amalgam. Alternative materials such as composite resins do not provide the clinical function for the length of time characteristically associated with dental amalgam. The weak link in the composite restoration is the dentin/adhesive bond. The purpose of this study was to correlate morphologic characterization of the dentin/adhesive bond with chemical analyses using micro-Fourier transform infrared and micro-Raman spectroscopy. A commercial dental adhesive was placed on dentin substrates cut from extracted, unerupted human third molars. Sections of the dentin/adhesive interface were investigated using infrared radiation produced at the Aladdin synchrotron source; visible radiation from a Kr+ laser was used for the micro-Raman spectroscopy. Sections of the dentin/adhesive interface, differentially stained to identify protein, mineral, and adhesive, were examined using light microscopy. Due to its limited spatial resolution and the unknown sample thickness the infrared results cannot be used quantitatively in determining the extent of diffusion. The results from the micro-Raman spectroscopy and light microscopy indicate exposed protein at the dentin/adhesive interface. Using a laser that reduces background fluorescence, the micro-Raman spectroscopy provides quantitative chemical and morphologic information on the dentin/adhesive interface. The staining procedure is sensitive to sites of pure protein and thus, complements the Raman results. © 1999 Society of Photo-Optical Instrumentation Engineers.

Change in temperature of subjacent bone during soft tissue laser ablation.

In tissues that closely approximate bone, sufficient heat may be transferred to the bone during laser surgery to cause damage and/or necrosis. To date, there have been few studies examining the temperatures elicited at the bone surface as a result of laser application to the overlying soft tissues. The purpose of this investigation was to determine, under in vitro conditions, temperature changes at the bone/soft tissue interface during laser ablation with CO2 and Nd:YAG lasers used with and without (w/wo) air/water coolant. Experimental specimens consisted of 5 mandibles from freshly sacrificed hogs; laser treatment sites were the buccal and lingual attached gingiva of the molars and the lingual keratinized mucosa of the incisor region. CO2 and Nd:YAG lasers were used w/wo coolant at power settings of 4 to 8 W and 5 to 9 W, respectively. Temperature changes were measured with a copper constant thermocouple contained within a 21 gauge hypodermic needle. In comparing the lasers at comparable energy densities w/wo coolant, temperature increases at the bone/soft tissue interface ranged from 8.0 to 11.1 degrees C with the Nd:YAG and 1.4 to 2.1 degrees C with the CO2. Similarly, in comparing the times required for the interface to return to baseline temperature following removal of the laser, values ranged from approximately 143 to 205 and approximately 119 to 139 seconds for the Nd:YAG and CO2, respectively. Results from this study suggest that, at energy densities equal or above those reported here, the increase in temperature at the bone surface as a result of periodontal soft tissue surgery with the Nd:YAG laser could be damaging, especially if the exposure is prolonged.

Equilibrium vapour pressure of mercury from dental amalgam under loading conditions.

Earlier studies have failed to establish a consensus on the amount of mercury vapour released from dental amalgam restorations. The purpose of this study was to accurately and quantitatively measure the equilibrium mercury vapour pressure from dental amalgam. The vapour pressure was measured using a quartz crystal microbalance as a function of the load from 0-5.4 MPa. Auger spectra were collected of the as-formed and argon ion sputter cleaned dental amalgam surface. For the as-formed surface the mercury vapour density is zero with no load and increases to 0.6 microg m(-3) at 5.4 M Pa. Following cleaning the mercury, vapour density increased to a maximum value of 15 microg m(-3). The Auger spectra of the as-formed surfaces were dominated by features associated with carbon and oxygen. These spectral results in concert with the mercury vapour density measurements indicate that the oxide film on the as-formed surfaces inhibited the release of mercury vapour. The results of this experiment provide an upper limit for the amount of mercury vapour released by dental amalgams. Under conditions simulating the oral cavity this value would be reduced by oxides that form on the surface of dental amalgam restorations.

Surface spectroscopy of apatitic materials: limitations and concerns.

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 effects of CO2 laser and Nd:YAG with and without water/air surface cooling on tooth root structure: correlation between FTIR spectroscopy and histology.

Morphologic and chemical characterization of root surfaces treated with either the CO2 laser, Nd:YAG, or Nd:YAG with water/air surface cooling (Nd:YAG-C) was completed using scanning electron microscopy (SEM) and FTIR photoacoustic spectroscopy (FTIR/PAS). Specimens for morphologic analysis consisted of 20 extracted single rooted teeth unaffected by periodontal disease. The specimens were exposed at varying energy densities to a single pass of the laser. SEM examination revealed, for all lasers, a direct correlation between increasing energy densities and depth of tissue ablation and width of tissue damage. The Nd:YAG-C required higher energy densities than either the CO2 or Nd:YAG lasers to achieve the same relative depth of tissue ablation. Regardless of energy density, and in contrast with other laser types, areas treated with the Nd:YAG-C did not exhibit collateral zones of heat damage. Specimens for spectroscopic examination consisted of 12 disks, 6 x 2 mm, cut from debrided root surfaces of extracted, unerupted human molars. The spectral results indicate a substantial reduction in the absorption bands attributable to protein and an additional band at 2015 cm-1 in specimens exposed to the Nd:YAG without water. In the presence of water/air coolant, the band at 2015 cm-1 appears only at a substanially higher energy density. The spectra of the CO2 treated specimens, with the char layer present, show a significant reduction in the protein bands and additional bands at 2015 and 2200 cm-1, that are tentatively assigned to the cyanamide and cyanate ions, respectively. These results suggest a reaction of the organic matrix and mineral with laser exposure.

Equilibrium vapor pressure of mercury from dental amalgam in vitro.

OBJECTIVES: The purpose of this study was to acquire reliable quantitative data on mercury vapor pressure above the surface of dental amalgam samples in both the as-formed and the abraded state. METHODS: The equilibrium vapor pressure of mercury from dental amalgam was obtained using residual gas analysis in conjunction with a quartz crystal microbalance. The measurements were performed under ultrahigh-vacuum conditions. RESULTS: Using the residual gas analyzer, the average mercury vapor pressures measured from the as-formed and abraded dental amalgam surfaces were 8 x 10(-7) and 1.7 x 10(-4) Pa, respectively. The corresponding vapor densities are: 6 x 10(-2) micrograms/m3 and 14 micrograms/m3. The average mercury vapor pressures measured from the as-formed and abraded dental amalgam surfaces using the quartz crystal microbalance were: 2.4 x 10(-6) and 1.0 x 10(-4) Pa, respectively. The corresponding vapor densities are: 0.2 microgram/m3 and 8 micrograms/m3. SIGNIFICANCE: This project provides a measurement of the equilibrium vapor pressure of mercury from as-formed and abraded amalgam surfaces. By definition, the equilibrium vapor pressure provides the maximum density of mercury which can be present in the environment above the amalgam. The vapor density of mercury within the oral cavity must be less than this value due to the dynamic nature of the system.

Wedge shaped cell for highly absorbent liquids: infrared optical constants of water.

We designed an improved wedge shaped cell for measuring Lambert absorption coefficient spectra alpha(nu) of highly absorbent liquids. The design allows for accurate determination of the apex angle of the wedge, sealing the cell, and injection of the liquid without disassembling the cell. We measured alpha(nu) for water through the 500-12,500-cm(-1) wavenumber region to determine the range of alpha(nu) for which the cell provided accurate measurements. We then determined the imaginary part of the complex refractive index N(nu) = n(nu) + ik(nu) from alpha(nu) and used Kramers-Kronig methods to compute n(nu) from k(nu).