• Restorative Dentistry and Endodontics
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• v.18 no.1
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• pp.73-83
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• 1993

The purpose of this study was to evaluate the effect of various acid treatments on dentin bonding. Freshly extracted human teeth were uprightly embedded in self curing acrylic resin, and their occlusal surfaces were grinded to expose flat dentin surfaces. The specimens were divided into 4 groups. Specimens of one group were not treated so as to be a control and those of the other three groups were threated with 10% polyacrylic acid, 10% phosphoric acid, and 10-3 solution(10% citric acid/3% ferric chloride) respectively. Primer, bonding resin and composite resin were applied over the treated dentin surfaces sequentially. All specimens were stored in $37^{\circ}C$ distilled water for 24 hours, then the tensile bond strength was measured and the treated dentin surfaces and fracured dentin surfaces were examined under a scanning electron microscope. The results were as follows: Bond strengths of acid-treated groups were higher than those of the untreated group. In the acid-treated groups, bond strength was found to be the highest in the 10-3 solution group followed by the 10% phosphoric acid group and the 10% polyacrylic acid group(P<0.01). On SEM examination of dentin surfaces, the untreated dentin surface showed a remaining smear layer and closed dentinal tubules. Dentin surfaces treated with 10 % polyacrylic acid showed a clean dentin surface without the smear layer, but showed remaining smear plugs in dentinal tubules. A dentin surface treated with 10% phosphoric acid or 10-3 solution showed open dentinal tubules without the smear layer or smear plugs. On SEM observation of the fractured dentin-resin interface, the untreated group showed that failure occurred in the smear layer. The group treated with 10% polyacrylic acid showed no resin tag remained in the dentinal tubules, but resin tags in the dentinal tubules were observed in the group treated with the 10% phosphoric acid or the 10-3 solution. On the failure mode examination, the higher the bond strength of the group, the higher the frequency of cohesive failure. The coefficient between bond strength and cohesive failure rate was 0.71.

• Journal of the korean academy of Pediatric Dentistry
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• v.26 no.4
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• pp.595-607
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• 1999

The purpose of this in vitro study was to evaluate the efficacy of self-etching primer which was developed to simplify the bonding procedures by measuring the shear bond strength and observing the interfacial morphology. 90 flat dentinal surfaces were prepared by grinding the buccal and lingual areas of caries-free human deciduous molars. After bonding of composite resin to sample surfaces according to the manufacturer's direction and thermocycling, shear bond strengths were measured using Universal testing machine(Instron). Another groups of specimens were treated by hydrochloric acid to secure the resin only and those tags were evaluated under SEM for their length and forms and the morphology of the bonding sites were also observed. The result as follows. 1. Group III showed higher shear bond strength than group I and II but no statistically significant difference was founded between group I and II(p>.05). 2. Adhesive failure was predominant in group II whereas dentin detachment was the main failure pattern in group I and III. 3. Relating long resin tags of $100-200{\mu}m$ were observed in samples of all groups under SEM. In group I, homogeneously long resin tags were arranged rather tight whereas rather loosely arranged resin tags of various length were found in group II. Lateral branching of resin tags was the characteristic finding observed in group III.

• Restorative Dentistry and Endodontics
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• v.20 no.1
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• pp.261-274
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• 1995

This study aimed to evaluate the marginal microleakage of Class V cavities of All-bond 2 (Wet - bonding system), Gluma (Adhesion of resin to exposed collagen fibers), and Scotchbond Multi-purpose(Mild Etching System). Hundred extracted human teeth divided into a control and three experimental groups consisting of eight teeth. The experimental group was further subdivided into All- bond2, Gluma and Scotchbond MP groups, Vitrebond served as the control. The positive control group consisted of specimens filled with resin and with no etching, primer and bonding procesure. Polished specimens underwent temperature changed from $5^{\circ}C$ to $55^{\circ}C$ a thousand times. After thermocycling, speciemens were placed in 2 % methylene blue dye solution for 24 hours in an incubator set at $37^{\circ}C$. The teeth were sectioned buccolingually and the degree of dye penetration was observed with a stereomicroscoped(*20). The following results were obtained. 1. Both the control and the experimental group showed a lower degree of dye penetration on enamel than on dentin margins(p<0.05) 2. Gluma exhibited a statistically significant lower degree of dye penetration than All-bond 2 on enamel margins(p<0.05) Scotchbond MP also exhibited a lower degree of dye penetration than All-bone 2 but was no statistically significant. Gluma and Scotchbond MP exhibited a similar degree of dye penetration. 3. The degree of dye penetration of All-bond 2, Gluma and Scotch bond MP showed no statistically singnificance on enamel margins but was significantly lower than in the control using Vitrebond. 4. All-bond 2 exhibited a statistically significant lower degree of dye penetration than Gluma on dentin margins. All- bond 2 and Scotchbond MP showed a similar degree of dye penetration. 5. The degree of dye penetration of All-bond 2, Gluma and Scotchbond MP showed no statistically significance on dentin margins. There was neither a statistical significance with the control.

• The korean journal of orthodontics
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• v.31 no.1 s.84
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• pp.137-147
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• 2001

Acidic primer is the bonding agent which combines the conditioning and priming agent into the single solution and was originally developed for the dentin bonding system. It is less harmful to the tooth structure and more convenient to manipulate than the traditional etching procedure. The Purpose of this study is to evaluate the shear bond strength of various bonding materials when the enamel is treated with acidic primer for the bracket bonding procedure. Fifty recently extracted human premolars were randomly separated into five groups -Group I using Clearfil Liner Bond 2 adhesive system to the enamel treated with acidic primer, Group II using Transbond XT adhesive system to the enamel treated with acidic primer, Group III using panavia 21 adhesive system to the enamel treated with acidic primer, Group IV using Fuji-Ortho LC adhesive system to the enamel treated with acidic primer, Group V using Transbond XT adhesive system to the enamel treated with 37$\%$ phosphoric acid. The shear bond strength was measured with Instron universal testing machine after storing in $37^{\circ}C$ water bath for 48 hours. After debonding, the teeth and brackets were examined under scanning electron microscope (SEM) and assessed with the adhesive remnant index (ARI). The results were as follows : 1. There were no significant differences in shear bond strength between group III ($8.69{\pm}2.72MPa$), group IV (9.7 ± 3.16 MPa), and group V ($10.48{\pm}2.60MPa$) (p>0.05). 2. The shear bond strength of group III and group IV was significantly higher than that of group I ($1.09{\pm}0.53MPa$), and Group II ($2.70{\pm}1.46MPa$) (p<0.05). 3. The ARI of group IV ($2.1{\pm}1.1$) and group V ($2.9{\pm}0.3$) was significantly higher than that of group I ($0.2{\pm}0.4$), group II ($0.3{\pm}0.9$) and group III ($0.2{\pm}0.4$) (p<0.05). 4. There were no significant difference between the ARI of group IV and group V (p>0.05). This result suggests that the combination of acidic primer and some bonding adhesive can provide sufficient shear bond strength for clinical orthodontics.

• Restorative Dentistry and Endodontics
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• v.20 no.1
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• pp.328-341
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• 1995

I. Shear Bond Strength to Air-dried and Remoistened Dentin.. The effect of air-drying and remoistening of acid-conditioned dentin before priming with the primer of All-Bond 2(BISCO. INC., U. S. A.) on shear bond strength(SBS) was investigated. Ninty freshly extracted sound human molars were divided at random into 9 groups of 10 teeth each. SBSs were meaured for acid-conditioned and non-conditioned dentin to which the primer and bonding agent of All-Bond 2 and composite resin(Z-100, 3M Dental Products, U. S. A.) were applied. The following values(Mean${\pm}$ SD, MPa) were obtained for the groups conditioned with 10% phosphoric acid for 15 seconds: Group l(blot dried) $6.7{\pm}4.1$ ; Group 2(10 seconds dried) $16.1{\pm}5.3$ ; Group 3(20 seconds dried) $15.4{\pm}4.8$ ; Group 4(30 seconds dried) $15.2{\pm}6.3$ ; Group 5(10 seconds dried/remoistened) $26.4{\pm}2.6$ ; Group 6(20 seconds dired/remositened) $22.2{\pm}2.7$ ; Group 7(30 seconds dried/remoistened) $21.5{\pm}4.1$. For the non-conditioned groups the values were: Group 8 (blot dried) $13.3{\pm}2.6$ ; Group 9(10 seconds dried) $12.9{\pm}3.5$. The data were analyzed using ANOVA. In the acid-conditioned groups, mean values of SBS for the air-dried specimens(Grps. 2, 3 and 4) and the 20 and 30 seconds dried/remoistened specimens (Grps. 6 and 7) were significantly lower than that of blot dried specimens.(p<0.05) The value for 10 seconds dried/remoistened specimens (Grp. 5), however, was not statistically different compared to that of blot dried specimens.(p>0.05) In the non-conditined groups, there was no statistical difference between blot dried and 10 seconds dried specimens.(p>0.05) The results suggest that the acid-conditioned dentin surface is more vulnerable to dentin bonding when it is air-dried or even remoistened after long period of drying. II. Shear bond stengh to the moistened and primed enamel. The effect of moistening and priming of enamel compared to the air-drying of enamel on the shear bond strength of enamel bonding agent was investigated. The experiment was divided into 4 groups each containing 10 caries-free maxillary incisor teeth. Shear bond strength values were measured for the primed and non-primed enamel to which All-Bond 2 and Z-100 were applied. The following values(MPa) were obtained for the primed groups pretreated with 32 % phosphoric acid for 15 seconds. : Group 1 (10 seconds dried) $29.8{\pm}2.2$ ; Group 2(moistened) $26.8{\pm}5.4$. For the non-primed groups the values were: Group 3(10 seconds dried/primed) $27.6{\pm}5.0$ ; Group 4(mostened/primed) $28.2{\pm}3.5$. The data were subjected to statistical analysis using ANOVA. The results showed that mean shear bond strengths among the experimental groups were not statistically different. (p>0.05) Conclusively, It is suggested that the bonding ability to enamel is not decreased by the moistening and priming of the enamel.

• Restorative Dentistry and Endodontics
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• v.25 no.1
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• pp.46-55
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• 2000

During bonding procedure of composite resin, the prepared cavity can be contaminated by saliva. In this study, marginal microleakage and shear bond strength of a composite resin to primed enamel and dentin treated with artificial saliva(Taliva$^{(R)}$) were evaluated. For the marginal microleakage test, Class V cavities were prepared in the buccal surfaces of fifty molars. The samples were randomly assigned into 5 groups with 10 samples in each group. Control group was applied with a bonding system (Scotchbond$^{TM}$ Multi-Purpose plus) according to manufacture's directions without saliva contamination. Experimental groups were divided into 4 groups and contaminated with artificial saliva for 30 seconds after priming: Experimental 1 group ; artificial saliva was dried with compressed air only, Experimental 2 group ; artificial saliva was rinsed and dried. Experimental 3 group ; cavities were etched with 35% phosphoric acid for 15 seconds after rinsing and drying artificial saliva. Experimental 4 group ; cavities were etched with 35% phosphoric acid for 15 seconds and primer was reapplied after rinsing and drying artificial saliva. All the cavities were applied a bonding agent and filled with a composite resin (Z-100$^{TM}$). Specimens were immersed in 0.5% basic fuschin dye for 24 hours and embedded in transparent acrylic resin and sectioned buccolingually with diamond wheel saw. Four sections were obtained from one specimen. Degree of marginal leakage was scored under stereomicroscope and their scores were averaged from four sections. The data were analyzed by Kruscal-Wallis test and Fisher's LSD. For the shear bond strength test, the buccal or occlusal surfaces of one hundred molar teeth were ground to expose enamel(n=50) or dentin(n=50) using diamond wheel saw and its surface was smoothed with Lapping and Polishing Machine(South Bay Technology Co., U.S.A.). Samples were divided into 5 groups. Treatment of saliva-contaminated enamel and dentin surfaces was same as the marginal microleakage test and composite resin was bonded via a gelatin capsule. All specimens were stored in distilled water for 48 hours. The shear bond strengths were measured by universal testing machine (AGS-1000 4D, Shimaduzu Co., Japan) with a crosshead speed of 5 mm/minute. Failure mode of fracture sites was examined under stereomicroscope. The data were analyzed by ANOVA and Tukey's studentized range test. The results of this study were as follows : 1. Enamel marginal microleakage showed no significant difference among groups. 2. Dentinal marginal microleakages of control, experimental 2 and 4 groups were lower than those of experimental 1 and 3 groups (p<0.05). 3. The shear bond strength to enamel was the highest value in control group (20.03${\pm}$4.47MPa) and the lowest value in experimental 1 group (13.28${\pm}$6.52MPa). There were significant differences between experimental 1 group and other groups (p<0.05). 4. The shear bond strength to dentin was higher in control group (17.87${\pm}$4.02MPa) and experimental 4 group (16.38${\pm}$3.23MPa) than in other groups, its value was low in experimental 1 group (3.95${\pm}$2.51 MPa) and experimental 2 group (6.72${\pm}$2.26MPa)(p<0.05). 5. Failure mode of fractured site on the enamel showed mostly adhesive failures in experimental 1 and 3 groups. 6. Failure mode of fractured site on the dentin did not show adhesive failures in control group, but showed mostly adhesive failure in experimental groups. As a summary of above results, if the primed tooth surface was contaminated with artificial saliva, primer should be reapplied after re-etching it.

• Restorative Dentistry and Endodontics
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• v.23 no.1
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• pp.141-161
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• 1998

The depth and patterns of demineralization according to the difference in concentration and application time of phosphoric acid were observed through the transmission electron microscope, and shear bond strengths to the acid -conditioned dentin were then measured and compared with the TEM results. To investigate the influence of polymer addition into the phosphoric acid and the effect of difference in concentration and application time of the acid, the specimens were randomly divided into 9 groups. Among the specimens, the exposed dentin surfaces were acid-conditioned with 10% polymer-thickened phosphoric acid(All Bond 2, Bisco, U.S.A.) and aqueous 10%, 20%, 30%, 40% phosphoric acid for 20 seconds, The rest of the specimens were acid-conditioned with 10% phosphoric acid for 15s, 30s, 60s, 120s respectively. The specimens were immersed in 4% glutaraldehyde in 0.1M sodium cacodylate buffer and postfixed with 1 % osmium tetroxide without decalcification and then observed under a JEOL Transmission Electron Microscope(JEM 1200 EX II, Japan). After the specimens were acid-conditioned as the above, primer and adhesive resin were applied to blot-dried dentin and shear bond strengths were then measured and analysed. The results were as follows : 1. The intertubular demineralization depth of 4.0-$5.0{\mu}m$ in 10% polymer-thickened phosphoric acid gels was similar or slightly deeper than that of 4.0-$4.5{\mu}m$ in aqueous 10% phosphoric acid solution. 2. The intertubular demineralization depth of aqueous 20%, 30% and 40% phosphoric acid solution was 6.5-$7.0{\mu}m$, 6.5-$7.5{\mu}m$ and 9.0-$15.0{\mu}m$ respectively. It showed that the depth of dentin demineralization is partly related to the concentration of phosphoric acid solution. 3. The intertubular demineralization depth of aqueous 10% phosphoric acid solution in application time for 15s, 30s, 60s and 120s was 2.5-$3.0{\mu}m$, 4.0-$6.0{\mu}m$, 6.5-$7.0{\mu}m$ and 8.5-$14.0{\mu}m$ respectively. It showed that the depth of dentin demineralization is directly related to the application time of phosphoric acid solution. 4. The partially demineralized dentin layer between demineralized collagen layer and unaffected dentin was showed to a width of 0.5-$1.0{\mu}m$ in lower concentration groups treated with aqueous 10% phosphoric acid for 20s, 60s, 120s and 20% phosphoric acid for 20s. 5. The demineralization effect at the border of intertubular-peritubular junction was less evident than that in the peritubular and intertubular dentin. The collagen fibers in the intertubular dentin had a random orientation, whereas those that lined the tubules were circumferentially aligned. The cross-linkage of dentinal collagen in demineralized collagen layer was clearly seen. 6. A statistically significant difference of bond strengths according to the difference in phosphoric acid concentration did not exist among the groups treated with 10%, 20%, 30% and 40% acid solution (P>0.05). However, bond strengths to the treated dentin with 10% phosphoric acid solution for 30s were significantly higher than that for 120s (P<0.05).

• Restorative Dentistry and Endodontics
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• v.24 no.4
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• pp.647-656
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• 1999

The purpose of this study was to investigate the shear bond strength and marginal microleakage of composite to enamel and dentin according to different treatment methods when the applied bonding agent was contaminated by artificial saliva. For the shear bond strength test, the buccal and occlusal surfaces of one hundred twenty molar teeth were ground to expose enamel(n=60) and dentin surfaces(n=60). The specimens were randomly assigned into control and 5 experimental groups with 10 samples in each group. In control group, a bonding system(Scotchbond$^{TM}$ Multi-Purpose plus) and a composite resin(Z-100$^{TM}$) was bonded on the specimens according to manufacture's directions. Experimental groups were subdivided into 5 groups. After polymerization of an adhesive, they were contaminated with at artificial saliva on enamel and dentin surfaces: Experimental group 1 ; artificial saliva was dried with compressed air. Experimental group 2 ; artificial saliva was rinsed with air-water spray and dried. Experimental group 3 ; artificial saliva was rinsed, dried and applied an adhesive. Experimental group 4 ; artificial saliva was rinsed, dried, and then etched using phosphoric acid followed by an adhesive. Experimental group 5, artificial saliva was rinsed, dried, and then etched with phosphoric acid followed by consecutive application of both a primer and an adhesive. Composite resin(Z-100$^{TM}$) was bonded on saliva-treated enamel and dentin surfaces. The shear bond strengths were measured by universal testing machine(AGS-1000 4D, Shimaduzu Co. Japan) with a crosshead speed of 5mm/minute under 50kg load cell. Failure modes of fracture sites were examined under stereomicroscope. The data were analyzed by one-way ANOVA and Tukey's test. For the marginal microleakage test, Class V cavities were prepared on the buccal surfaces of sixty molars. The specimens were divided into control and experimental groups. Cavities in experimental group were contaminated with artificial saliva and those surfaces in each experimental groups received the same treatments as for the shear test. Cavities were filled with Z-100. Specimens were immersed in 0.5% basic fuchsin dye for 24 hours and embedded in transparent acrylic resin and sectioned buccolingually with diamond wheel saw. Four sections were obtained from the one specimen. Marginal microleakages of enamel and dentin were scored under streomicroscope and averaged from four sections. The data were analyzed by Kruskal-Wallis test and Fisher's LSD. The results of this study were as follows. 1. The shear bond strength to enamel showed lower value in experimental group 1(13.20${\pm}$2.94MPa) and experimental group 2(13.20${\pm}$2.94MPa) than in control(20.03${\pm}$4.47MPa), experimental group 4(20.96${\pm}$4.25MPa) and experimental group 5(21.25${\pm}$4.48MPa) (p<0.05). 2. The shear bond strength to dentin showed lower value in experimental group 1(9.35${\pm}$4.11MPa) and experimental group 2(9.83${\pm}$4.11MPa) than in control group(17.86${\pm}$4.03MPa), experimental group 4(15.04${\pm}$3.22MPa) and experimental group 5(14.33${\pm}$3.00MPa) (p<0.05). 3. Both on enamel and dentin surfaces, experimental group 1 and 2 showed many adhesive failures, but control and experimental group 3, 4 and 5 showed mixed and cohesive failures. 4. Enamel marginal microleakage was the highest in experimental group 1 and there was a significant difference in comparison with other groups (p<0.05). 5. Dentin marginal microleakages of experimental group 1 and 2 were higher than those of other groups (p<0.05). This result suggests that treatment methods, re-etching with 35% phosphoric acid followed by re-application of adhesive or repeating all adhesive procedures, will produce good effect on both shear bond strength and microleakage of composite to enamel and dentin if the polymerized bonding agent was contaminated by saliva.

• Restorative Dentistry and Endodontics
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• v.32 no.4
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• pp.327-334
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• 2007

The purpose of this study was to evaluate the effect of burs on microleakage of Class V resin restorations when a self-etching primer adhesive was used. Forty Class V cavities were prepared with four different cutting burs on extracted third molars, and divided into one of four equal groups (n = 10); Group 1-plain cut carbide bur (no. 245), Group 2-cross cut carbide bur (no. 557), Group 3-fine diamond bur (TF-21F), Group 4-standard diamond bur (EX-41). The occlusal and gingival margin of cavities was located in enamel and dentin, respectively. Cavities were treated with Clearfil SE Bond and restored with Clearfil AP-X. Specimens were thermocycled, immersed in a 2% methylene blue solution for 24 hours, and bisected longitudinally. They were observed leakages at enamel and dentinal margins. Data were analyzed using Mann-Whitney and Wilcoxon signed ranked test. The results of this study were as follows; 1. At enamel margin, microleakage of group 4 was statistically higher than those of group 1, 2 and 3 (p < 0.01). 2. At dentinal margin, microleakage of group 4 was statistically higher than group 3 (p < 0.01), but group 1 and 2 were not statistically different with group 3 and 4. 3. Enamel microleakage was statistically higher than dentinal microleakage in group 1, 2 and 3 (p < 0.05), but statistical difference between the microleakage of enamel and dentinal margin was not in Group 4. In conclusion, the use of coarse diamond bur showed high microleakage at both enamel and dentinal margin when Clearfil SE Bond was used in class V cavity.

• Restorative Dentistry and Endodontics
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• v.24 no.1
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• pp.147-155
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• 1999

The purpose of this study was to investigate the effect of phosphoric acid concentration on the movement of 2-hydroxyethylmethacrylate(HEMA) from bonding resin - resin composite combination through dentin in vitro. Freshly extracted human third molar teeth were divided into four groups each of 10 teeth. A closed chamber with 1 ml distilled water was attached to the CEJ of each tooth. An occlusal cavity of 4mm diameter & remaining dentin thickness of 1.0-1.5mm was prepared in each tooth. Dentin was treated with 10% phosphoric acid gel for 15 seconds. 32% phosphoric acid gel for 15 seconds, or with 35% phosphoric acid gel for 15 seconds. A control group not treated with acid gel was also prepared. The cavities were rinsed, dried and then treated with the HEMA-containing All-Bond 2 primer & bonding resin which was light-cured for 10 seconds. The cavities were then restored with Z100 composite resin(shade:A3.5:3M Dent. Prod. USA) & light cured for 30 seconds. Water samples were retrieved from the chambers over a time course (4.32, 14.4, 43.2, 144 & 432 minutes ; 1, 3 & 10 days) and analyzed by high performance liquid chromatography. The results were as follows. 1. HEMA was detected in the pulp chambers of all teeth from 4.32 minutes after resin placement The highest rate of release was in the first sample period (0-4.32 min) & rate of release declined exponentially thereafter. 2. No significant differences were found for mean release rate for HEMA over a time course among the four groups (p>0.05). 3. The diffusion rate was significantly (p<0.05) less for 10% phosphoric acid gel than 32% phosphoric acid gel at the second sample period(4.32-14.4 min). 4. No significant differences were found for cumulative HEMA diffusion among the four groups at 10 days(p>0.05) and mean total(cumulative) release at 10 days for all groups was in the 9 - 16 nmol range. 5. The cumulative release was significantly (p<0.05) less for 10% phosphoric acid gel than 32% phophoric acid gel at the third(14.4-43.2 min) & fourth(43.2-144 min) sample period.