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RESEARCH REPORTS

Biomaterials & Bioengineering

C.K.Y. Yiu1, N.M. King1, B.I. Suh2,
L.J. Sharp2, R.M. Carvalho3,
D.H. Pashley4, and F.R. Tay1*
1 Paediatric Dentistry and Orthodontics, Faculty of
Dentistry, The University of Hong Kong, 34 Hospital Road,
Hong Kong SAR, China; 2Bisco Inc., Schaumburg, IL,
USA; 3Department of Operative Dentistry, Endodontics and
Dental Materials, Bauru School of Dentistry, University of
São Paulo, Bauru, SP, Brazil; and 4Department of Oral
Biology and Maxillofacial Pathology, School of Dentistry,
Medical College of Georgia, Augusta, GA, USA;
*corresponding author, kfctay@netvigator.com

Incompatibility of Oxalate
Desensitizers with Acidic,
Fluoride-containing
Total-etch Adhesives

J Dent Res 84(8):730-735, 2005

ABSTRACT

INTRODUCTION

The use of oxalate desensitizers on acid-etched
dentin prior to adhesive application can result in
subsurface tubular occlusion by calcium oxalate
crystals. However, the solubility of calcium
oxalate increases in acidic solution. We
hypothesized that total-etch adhesives can,
depending upon their pH, interact with oxalatedesensitizer-treated dentin in an adverse manner.
Acid-etched human dentin treated with 2 oxalate
desensitizers (BisBlock and Super Seal) was
bonded with 4 simplified total-etch adhesives:
One-Step (OS), Single Bond (SB), OptiBond Solo
Plus (OB), and Prime&Bond NT (PB).
Composite-dentin beams were examined by SEM
and TEM, both of which revealed numerous
spherical globules on OB- and PB-bonded,
desensitizer-treated dentin, but not in OS or SB
samples. Bond strengths produced by OB and PB
were significantly lower in oxalate-treated
specimens than those produced by OS or SB.
These surface globules may have interfered with
hybridization of demineralized dentin with OB
and PB resins and caused compromised bond
strengths.

sensitivity is frequently encountered with the use of
P2001;ost-operative
adhesives that require the acid-etching of vital dentin (Akpata and Sadiq,
Unemori et al., 2001). The application of these total-etch adhesives

KEY WORDS: oxalate desensitizer, acid-etch,
single-bottle adhesives, pH, fluoride.

Received August 27, 2004; Last revision May 12, 2005;
Accepted May 13, 2005
A supplemental appendix to this article is published
electronically only at http://www.dentalresearch.org.

730

can be technique-sensitive, since wet bonding is required for full expansion
and optimal hybridization of the demineralized collagen matrix (Gwinnett,
1992; Kanca, 1992). The difficulty in bonding is further complicated by the
intrinsic wetness of vital deep dentin after removal of the smear layer
(Itthagarun and Tay, 2000), and the increased permeability associated with
the simplified version of these adhesives (Tay et al., 2003a). Incomplete
sealing and continuous transudation of dentinal fluid through open dentinal
tubules before polymerization of the adhesive may result in entrapment of
water-filled blisters along the adhesive interface (Tay et al., 1996).
Compression of these blisters during mastication may cause, within the
dentinal tubules (Brännström and Johnson, 1970), rapid fluid movement that
activates the intradental A␦ nerve fibers (Närhi et al., 1994), which results
in post-operative sensitivity.
One way of relieving post-operative sensitivity clinically is the
adjunctive use of oxalate desensitizers on acid-etched dentin prior to
adhesive application (Pashley et al., 2001; Tay et al., 2003b). Depletion of
calcium ions from the surface dentin forces the oxalate ions to diffuse
further down into the dentinal tubule, until calcium ions are encountered for
reaction. The calcium oxalate crystals that are formed result in subsurface
tubular occlusion and reduction in the hydraulic conductance of dentin.
However, the solubility of calcium oxalate is affected by pH, since the anion
is the conjugate base of a weak acid (Kotz and Treichel, 1999). Preliminary
screening of the compatibility of oxalate desensitizers with total-etch
adhesive systems revealed complete compatibility with One-Step (Bisco)
and Single Bond (3M ESPE) and poor compatibility with Prime&Bond NT
(Dentsply) and OptiBond Solo Plus (Kerr). This led to a more detailed
investigation seeking the reasons for compatibility vs. incompatibility. The
purpose of this study was to determine if the acidity of total-etch adhesives
may influence their bonding to oxalate-desensitizer-treated acid-etched
dentin.
Thus, the objectives of this study were: (1) to compare the microtensile
bond strengths of 4 single-bottle total-etch adhesives of different acidities to
oxalate-desensitizer-treated acid-etched dentin; and (2) to examine, with the
use of scanning and transmission electron microscopy, the ultrastructure of
the bonded interface. The null hypothesis tested was that there is no
difference in the bonding of single-bottle total-etch adhesives of different
acidities to oxalate-desensitizer-treated acid-etched dentin.

Downloaded from jdr.sagepub.com at Uni Latinoamericana PARENT on September 24, 2016 For personal use only. No other uses without permission.
International and American Associations for Dental Research

Three readings were taken for each adhesive. Since the ␮ TBS data were not normally distributed (Kolmogorov-Smirnof test). Super Seal was applied with a rubbing motion for 30 sec and rinsed with water for 60 sec before bonding occurred. and were examined. CA. Five restored teeth were used for microtensile bond strength evaluation and 2 teeth for ultrastructural examination..81 2.9-mm slabs. UK).. IL. Schaumburg. USA). Kerr Co. Bisco Inc.. Beverly. unstained.9 (6.) and Super Seal (SS. Paul. operating at 10-20 kV.60 2. Groups identified with the same superscripts are not significantly different (p > 0.8 (6.1)a [ 0/40] 12. Phoenix Dental Inc. Dentsply De Trey. MN.. the silver-impregnated slabs were processed for transmission electron microscopy (TEM) without further demineralization.7 (4. Composite build-ups were performed with the use of a light-cured composite (Z250. coronal dentin. Canton.9-mm compositedentin beams (Shono et al.5)a [0/40] 43.2)a [0/40] 49. To circumvent this problem. The Table.8)a [ 0/40] 40.J Dent Res 84(8) 2005 Incompatibility of Oxalate Desensitizers MATERIALS & METHODS Eighty-four non-carious human third molars. International and American Associations for Dental Research . we dispensed 2-mL specimens of each adhesive into clean glass vials containing 3 mL of 70% ethanol and 30% distilled water. USA. Downloaded from jdr.4 ( 4. Model 4440 (Instron. according to the silver impregnation protocol reported by Tay et al.6)b [ 8/40] 6.3)a [0/40] 51. no desensitizer) BisBlock (BB) plus Adhesive Super Seal (SS) plus Adhesive 4. Bisco Inc.05). OptiBond Solo Plus (OB. Orange.6 ( 8. Specimens were 731 stressed to failure under tension in a Bencor Multi-T device (Danville Engineering. Beams with premature bond failure were assigned a null bond strength value and were included in the compilation of the mean bond strength. The 3 experimental groups were: Group 1: The surface to be bonded was etched with a 32% phosphoric acid gel (Uni-Etch. Transmission Electron Microscopy Two teeth from each group were acid-etched and similarly treated with the oxalate desensitizers in the manner as previously described. Group 3: After the surface was acid-etched. The data collected were analyzed with SigmaStat Version 2.6 ( 8. The teeth were sectioned into 0. BisBlock was applied with a rubbing motion for 30 sec and rinsed with water for 60 sec before bonding occurred. Bisco Inc. USA) with the use of a universal testing machine. coated with gold/palladium. Lake Bluff.sagepub.8 (4. The teeth were collected after the patients' informed consent had been obtained under a protocol approved by the Institutional Review Board of the Medical College of Georgia. Bonded surfaces were air-dried and light-cured for 10 sec. Experimental Design Four single-bottle total-etch adhesives and 2 oxalate desensitizers were investigated. Buehler Ltd. ␮TBS) Microtensile Bond Strength (␮ Bonding was performed on the occlusal surfaces of deep.2 (7. The Netherlands) at 80 kV.68 70 130 4527 3641 48. The oxalate desensitizers were: BisBlock (BB.9 (10.05.1 (9. MI. Fenton. Beams with premature failure during specimen preparation were included as null bond strengths in the calculation of mean bond strength. Each adhesive was divided into 3 experimental groups with 7 teeth each. Five teeth from each group yielded 40 beams for bond strength evaluation. 3M ESPE) in 5 1-mm increments and individually light-cured for 40 sec. USA). Single Bond (SB.8)a [ 0/40] 39. USA). 1999). IL. Measurement of pH and F Concentration of Adhesives Water-free adhesives that are dissolved in polar solvents do not usually dissociate into ionic species. They were immersed in a 50 wt% ammoniacal silver nitrate solution for 24 hrs.. with statistical significance set at ␣ = 0. Chicago. Philips. (2002).) for 15 sec and rinsed with water for 20 sec before bonding occurred. pH Values and F Concentrations of the 4 Total-etch. USA). USA) under water cooling.9 x 0. were used within 1 mo following extraction. Similarly to the pH measurement.6)b [12/40] 47.. by TEM (Philips EM208S.1 (4. and examined with a SEM (Cambridge Stereoscan 440. the data were analyzed by Kruskal-Wallis one-way ANOVA on ranks and Dunn's multiple-comparison tests.03 (SPSS. San Ramon. USA). 3M ESPE. Two-step Adhesives and Their Microtensile Bond Strengths after Bonding to Oxalatedesensitizer-treated Acid-etched Dentin Microtensile Bond Strength (MPa)1 Adhesives One-Step (OS) Single Bond (SB) OptiBond Solo Plus (OB)2 Prime&Bond NT (PB)2 1 2 pH F Concentration (ppm F) Control (adhesive only. Bonded teeth were then sectioned occluso-gingivally into 0.5% chloramine T solution at 4°C. and the mean pH value was calculated for each adhesive.4 (4. The dentin sides of the fractured specimens were air-dried. CA.60 3. Scanning Electron Microscopy Four representative fractured beams from each group with ␮TBS close to the mean bond strength of that group were selected for fractographic analysis by scanning electron microscopy (SEM). Augusta. Germany). MA. USA). USA). The treated teeth were bonded according to the manufacturers' instructions. The 2 widest slabs were coated with 2 layers of nail varnish applied 1 mm from the bonded interfaces. and Prime&Bond NT (PB. Eindhoven. A 180-grit silicon carbide paper was used under running water to create a clinically relevant smear layer on the dentin surface. Konstanz. Eight beams were retrieved from the 2 widest slabs of each tooth. a 2-mL specimen of each simplified-step adhesive was dispensed into a clean glass vial containing 3 mL of 70% ethanol and 30% distilled water.0)b [14/40] Values are means ± standard deviation [N = 40]. Inc. MA. After reduction of the diamine silver ions. Cambridge. that were stored in a 0. Orion Research. IL. at a crosshead speed of 1 mm/min. 2016 For personal use only. No other uses without permission. The adhesives were: One-Step (OS. Inc. The occlusal enamel was removed with the use of a slow-speed saw with a diamond-impregnated disk (Isomet. The pH values of the 4 adhesive solutions were measured at ambient temperature (22-25°C) by means of a digital pH meter (Model 501.6)a [ 0/40] 16. Group 2: After the surface was acid-etched.2)a [0/40] 47.com at Uni Latinoamericana PARENT on September 24. St.8)b [ 5/40] 5.. The teeth were stored in distilled water at 37°C for 24 hrs.

solution was buffered with TISAB III (Orion Research Inc. In contrast. No major differences could be recognized between the 2 oxalate desensitizers after the application of OB and PB.. Spherical globules could also be seen in the voids of the adhesive layers of PB-BB (Fig. These spherical globules closely resemble the loosely bound spherical calcium fluoride (CaF2)like material formed on enamel (Dijkman et al. SB and OS showed no significant differences in bond strength when applied to oxalate-treated and untreated acid-etched dentin (p > 0. Since both the microtensile bond strengths and ultrastructural features of the simplified total-etch adhesives were different when bonded to oxalate-desensitizertreated acid-etched dentin. Discontinuous spaces with scalloped margins were found between the hybrid and adhesive layers in OB-BB. The dentinal tubules were filled with silver deposits. In contrast to OB and PB. Table). The bond strengths of OS and SB were not compromised with the adjunctive use of the oxalate desensitizers. No. with no subsurface oxalate crystals identified. The results of this study showed that effective bonding to the desensitizer-treated acid-etched dentin is adhesive-specific. Nanoleakage was also observed within the entire hybrid layer from OB-BB (Fig. Better sealing ability of conventional three-step total-etch and two-step self-etch adhesives (De Munck et al. 1C). Clusters of smaller globules (arrow) were found between the larger globules. Frankenberger and Tay. since this clinical complication is highly product-related. and no spherical globules were seen (Fig. 3). 2005. In contrast. 96. Patent dentinal tubules (pointer) were frequently observed. the failure mode of the SB and OSoxalate subgroups was predominantly "mixed". These crystals can be seen more clearly in cryofractured specimens (Fig. 2-4 ␮m) located preferentially at the orifices of the dentinal tubules. (A) Spherical globules (arrowheads) with sizes ranging from 2 to 4 ␮m were preferentially found at the orifices of the dentinal tubules in the PB-SS subgroup. The fluoride concentrations were determined at ambient temperature by an ion-selective electrode (Cat. (D) No spherical globules could be found on the dentin surface of the SB-SS subgroup. (C) The dentin side of the OB-BB subgroup was covered with a continuous layer of spherical globules with sizes ranging from 0. Optimal resin infiltration and hybrid layer formation occurred in the presence of bi-pyramidal calcium oxalate dihydrate crystals in the dentinal tubules. respectively. International and American Associations for Dental Research .com at Uni Latinoamericana PARENT on September 24. Orion Research Inc. and electronlucent spherical globules with silver deposits were observed in the adhesive layer. TEM Results Figure 1. SEM micrographs of the dentin side of a fractured beam following application of singlebottle total-etch adhesives to oxalate-desensitizer-treated acid-etched dentin. No statistically significant difference was noted between BisBlock and Super Seal when used with the 4 adhesives.)..). 732 J Dent Res 84(8) 2005 Fluoride Analysis Ion-specific fluoride analysis of the 4 adhesive systems revealed relatively low levels in OS and SB (70 and 130 ppm. 2B). In contrast. RESULTS Microtensile Bond Strength The ␮TBS of the 4 adhesives. that could be attributed to the presence of spherical globules along the adhesive-dentin interface.Yiu et al. we have to reject the null hypothesis tested. Table). 1983. 1A). 2016 For personal use only. 2A). and their measured pH values and F concentrations are summarized in the Table. DISCUSSION The application of oxalate desensitizers to acid-etched dentin prior to adhesive application represents one way of avoiding post-operative sensitivity.sagepub. compared with very high levels in OB and PB (4527 and 3641 ppm. The dentin surfaces were characterized by spherical globules (diameter. isolated silver deposits were found in only some areas of the hybrid layer of SB-SS (Fig. Similarly to PB. 2005) may similarly block the effects of hydraulic pressure and reduce post-operative sensitivity. SEM Results Adhesive failure occurred predominantly along the adhesivedentin interface in PB-SS (Fig. Both OB and PB showed significant reduction in ␮TBS when applied to oxalate-treated acid-etched dentin (p < 0. Numerous fractured resin tags (arrowheads) could be seen at the base of the hybrid layer (H).05). 2C) and OS-BB (Fig. 2D). Bonded interfaces from PB-SS specimens revealed extensive nanoleakage of silver within the hybrid layer. (B) Spherical globules (pointers) up to 12 ␮m were also observed in the adhesive layer of the PB-BB subgroup. Nelson Downloaded from jdr. 1D). Patent dentinal tubules (arrowheads) were evident from the dentin (D) below. Discontinuous electronlucent spaces could be identified along the adhesive-dentin interface (Fig. No other uses without permission. numerous spherical globules were evident on the fractured dentin surfaces of OBBB (Fig.05). 1B).5 to 3 ␮m. significantly lower bond strengths were observed in OB and PB when applied to oxalate-desensitizer-treated dentin.

(C) A high-magnification view of greater intensity of fluoride deposition the hybrid layer in the SB-BB subgroup. Silver and OB are fluoride-containing deposits were occasionally seen within the spherical globules.sagepub. No surface globular structures could be identified. Both PB (T). and dentin specimens that were bonded with single-bottle total-etch adhesives. (D) A globular structures were formed high-magnification view of subsurface angular crystalline deposits (asterisk) within the dentinal tubule (T) in the OS-BB subgroup. Regardless of the composition of the spherical globules found on the surfaces of oxalatetreated specimens bonded with the 2 incompatible adhesive systems (OB and PB). The globules (pointer).. 1988. 1983. International and American Associations for Dental Research . Unstained. 2002) following topical fluoride treatment.. A: adhesive. could be identified along the adhesive-dentin interface..com at Uni Latinoamericana PARENT on September 24. Variability was seen in size and distribution densities of these globular structures following the application of PB and OB to oxalate-desensitizertreated dentin. 1984) and demineralized dentin surfaces (Itota et al.J Dent Res 84(8) 2005 Incompatibility of Oxalate Desensitizers 733 et al.. the calcium ions could oxalate-treated dentin. to oxalate-treated dentin. The dentinal tubules (beneath the position of the hybrid layer) were blocked by subsurface PB (3641 ppm. where extensive surface is also critical. TEM examination of the bonded interface also revealed discontinuous electronlucent spaces with distinct "scalloped" margins. U: undemineralized dentin. The bonded specimens were immersed in an ammoniacal silver nitrate tracer solution before laboratory dehydration and the availability of calcium ions on the epoxy resin embedding. Since the dentin surface was completely accumulation of silver deposits was observed in the porous deprived of calcium phosphate following phosphoric-acidhybrid layers following the application of PB and OB to etching (Van Meerbeek et al. oxalate (CaC2O4) is affected by pH. Similar effects have recently been have been derived from the dissolution of calcium oxalate reported following the application of hydrofluoric acid gel to crystals in the dentinal tubules. Only isolated spots of silver grains (arrowhead) were in OB may be explained by the higher observed in the hybrid layer (H). The presence of spherical globules on the surface of the desensitizer-treated dentin may hinder formation of the spherical globules in OB.and PB-bonded the adhesive infiltration and hybridization of demineralized specimens. dentin surface (Arends et al. with scalloped margins resembling conglomerates of spherical to precipitate CaF2-like material. it is reasonable to assume with a scalloped margin could be identified along the adhesive-hybrid layer interface (open arrow). 2000. No other uses without permission.. Conversely. These spherical globules were removed by the KOH extraction method (Caslavska et al.. since they were not infiltrated by silver deposits. 1988). since the anion is the Although the presence of fluoride ion is necessary for Downloaded from jdr. layer. since these adhesives contain minimum amounts of fluoride (Table). their presence at the bonded interface and in the adhesive layer could serve as stress-raisers that would create debonding at lower stresses than would occur in their absence. 2003). (B) A specimen from the adhesives may interact with calcium OB-BB subgroup. no electronlucent deposits (asterisk). The "scalloped" margins correlated nicely with the shapes of spherical globules. (A) A specimen from the PB-SS subgroup. probably representing the calcium oxalate crystals (arrow). showing extensive nanoleakage (open arrowheads) in the hybrid layer (H) and the dentinal tubule Saxegaard and Rölla. showing fairly extensive nanoleakage (arrowhead) within the hybrid layer (H). 2016 For personal use only. This could be due to the differences in concentration of Figure 2. and phosphate ions on dentin surfaces Discontinuous electronlucent deposits. The solubility of calcium acid-etched dentin (Szep et al. undemineralized TEM micrographs of oxalate-desensitizer-treated acid-etched fluoride. 2003). P: polyalkenoic acid copolymer component of the adhesive. Discontinuous electronlucent structures adhesives. Electronlucent crystals. This is supported by the TEM results. No globular structures were identified on the surface of the hybrid F concentration in OB (4527 ppm) vs. Silver deposits following the application of OS and SB (arrowhead) were occasionally observed within the hybrid layer (H). Pioch et al. Electronlucent spherical globules (pointer) were depicted in the adhesive layer (A). the availability of calcium ions on the dentin dentin. Table). confirming that the globules were KOH-soluble fluoride (Appendix). were also seen in that the free fluoride ions from the the dentinal tubules at a position that was 8-10 ␮m from the dentin surface. 1975). pH values of PB and OB. These were not true gaps along the adhesive-dentin interfaces.. Subsurface electronlucent deposits (asterisk) were also observed in the dentinal tubules (T).

Clinicians should be aware of the potential drop in bond strength with the use of PB and OB on oxalate-desensitizer-treated acid-etched dentin. Principles of reactivity: precipitation reactions. (2005). Tay FR (2001). at 8-10 ␮m beneath the dentin surface. by grants DE 014911 and DE 015306 from the National Institute of Dental and Craniofacial Akpata ES.. Dijkman TG (1988). the University of Hong Kong. The other authors have no financial interest in any of the products.Yiu et al. as calcium oxalate crystals are exposed to more H3O+. conjugate base of a weak acid. 4th ed. Self-etch vs etch-and-rinse adhesives: effect of thermo-mechanical fatigue loading on marginal quality of bonded resin composite restorations. for technical assistance. Faculty of Dentistry.I. In vivo investigation on the fluoride content in and on human enamel after topical applications. Inc. Moist versus dry dentin: its effect on shear bond strength. 'Calcium fluoride-like' material formed in partially demineralized human enamel in vivo owing to the action of fluoridated toothpastes. Pereira JC. 2003). Brazil. In: Chemistry and chemical reactivity. Närhi M. An in vitro study.. Gwinnett AJ (1992). TX: Saunders College Pub. the company that manufactures BisBlock. Caries Res 17:392-402. Dorfer CE. Arends J (1983). to compensate for the depletion of oxalate ions and maintain the equilibrium constant. Bonding to dentin. Effect of fluoride application on tensile bond strength of self-etching adhesive systems to demineralized dentin. In contrast. Resin bonding to wet substrate. Itthagarun A. Reintsema H. the oxalate desensitizer used in this study. Garcia-Godoy F. Acta Odontol Scand 28:59-70. Nelson DG. Inc. Itota T. Yoshiyama M (2002). Nelson DG. Treichel P (1999). J Dent Res 63:6-12. Peumans M. International and American Associations for Dental Research . Fort Worth. Staehle HJ (2003). USA (P. SEM micrograph of cryofractured phosphoric-acid-etched dentin following the application of an oxalate desensitizer. Quintessence Int 23:39-41. A critical review of the durability of adhesion to tooth tissue: methods and results. De Munck J. 2016 For personal use only. the etched dentin surface was devoid of the spherical calcium-fluoride-like structures. J Prosthet Dent 88:503-510. and to Jenny Wang of Bisco Inc. Surface characteristics of dentin experimentally exposed to Downloaded from jdr. In conclusion. Arch Oral Biol 20:333-339. Brännström M. Crystallographic structure of enamel surfaces treated with topical fluoride agents: TEM and XRD considerations. Johnson G (1970). and smaller. Byoung Suh is President of Bisco. Gotz H. Jongebloed WL. Arch Oral Biol 39(Suppl):23S-30S. J Dent Res 62:1201-1208.. Only demineralized collagen fibrils (pointer) were identified from the surface of the acid-etched dentin. Arends J (1984). This study was supported by RCG CERG grant 10204604/07840/08004/324/01. Poitevin A. Pioch T. Am J Dent 14:34-38. Sadiq W (2001). Tay FR (2000). Lambrechts P. Dent Mater 21:397-412. the University of Hong Kong. No other uses without permission. pp. calcium oxalate crystals in the dentinal tubules following the application of OB and PB to oxalate-desensitizer-treated dentin. J Dent Res 84:118132. Drs. Torii Y. David Pashley). Post-operative sensitivity in glassionomer versus adhesive resin-lined posterior composites. Brudevold F (1975).com at Uni Latinoamericana PARENT on September 24. 734 J Dent Res 84(8) 2005 Research. The use of oxalate to reduce dentin permeability under adhesive restorations. Pashley DH. de Boer P. In vivo studies are needed to confirm these in vitro observations. Caslavska V. the demineralized collagen matrix (asterisk) was almost completely devoid of these angular crystals. Movements of the dentine and pulp liquids on application of thermal stimuli. 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