Effect of temperature on water sorption and solubility of dental adhesive resins

Objective

This study examined the effect of temperature on water sorption and solubility characteristics of four commercial dental adhesives. The null hypothesis tested was that temperature has no effect on the water sorption and solubility characteristics of these adhesives.

Methods

The tested materials were: three-step etch-and-rinse (All-Bond 2, AB), two-step etch-and-rinse (One-Step, OS), two-step self-etch (Clearfil SE Bond, SE) and one-step self-etch (Clearfil S3 Bond, S3) adhesives. Seven resin disks (6 mm in diameter × 1 mm in thickness) were prepared from each tested material and were stored in deionized water at 23 °C, 37 °C and 55 °C. Water sorption and solubility of the resin disks were measured before and after water immersion and desiccation following two consecutive sorption and desorption cycles. The water sorption and solubility values obtained were analyzed using two-way ANOVA and Tukey's multiple comparison tests. The relationships between maximum water sorption, solubility and kinetics of water diffusion with temperature were evaluated by means of Pearson correlation statistic.

Results

OS exhibited the highest water sorption and solubility values in the second sorption–desorption cycle at 55 °C (p < 0.001). This is followed by S3, SE and AB with no significant difference between SE and AB. Significant positive correlations were observed between maximum water sorption (r = 0.307, p < 0.01), solubility (r = 0.244, p < 0.05), water sorption (r = 0.651, p < 0.001) and desorption (r = 0.733, p < 0.001) diffusion coefficients (obtained using Fick's law of diffusion) with temperature in the second cycle.

Significance

High temperatures increased water sorption of simplified adhesives. Such water sorption may contribute to the failure of resin–dentin bonds.     

3种一步法自酸蚀粘接剂固化后的吸水性和溶解性

目的 比较3种市售的一步法自酸蚀粘接剂的吸水性及溶解性,为临床操作提供指导.方法 选择3种一步法自酸蚀粘接剂Adper Easy Bond (AEO)、Optibond All-in-one (OP)和BeautiBond (BB),各制备50个圆盘试件(直径为8.0mm,厚度为1.0mm),浸泡于去离子水中,并分组于不同浸泡时间段(1天、7天、30天、90天、180天),通过浸水前后质量变化测定其吸水值与溶解值.结果 在每个浸泡期,OP的吸水值、溶解值均为最高,AEO吸水值居中、溶解值最低,BB吸水值最低而溶解值居中,不同品牌粘接剂组间比较,差异均有统计学意义(P＜0.05);3种粘接剂的溶解值均随时间延长显著增加,不同浸泡时间组内比较,差异均有统计学意义(P＜0.05).结论 3种市售的一步法自酸蚀粘接剂固化后的吸水性和溶解性明显不同,可能与其组成有关.     

Use of Hoy's solubility parameters to predict water sorption/solubility of experimental primers and adhesives

Self-etching primers and adhesives contain very hydrophilic acidic monomers that result in high water sorption/solubilities of their polymers. However, the chemical composition of these products varies widely. The purpose of this work was to vary the chemical composition of experimental self-etching primers and adhesives to determine if the water sorption/solubility of the polymers were affected in a predictable manner. The Hoy's solubility parameters of these mixtures were calculated to permit ranking of the degree of hydrophilicity of the polymers. Water sorption/solubility was measured according to ISO 4049. The results showed highly significant (R(2) = 0.86, P < 0.001) correlations between water sorption and Hoy's solubility parameter for polar forces (delta(p)) of the polymers. Similar correlations were obtained between polymer solubility and delta(p). When these results were compared with previously published results obtained with more hydrophobic resins, excellent correlations were obtained, indicating that Hoy's delta(p) values may be used to predict the water sorption behavior of methylmethacrylate polymers.     

Long-term evaluation of water sorption and ultimate tensile strength of HEMA-containing/-free one-step self-etch adhesives

Objective

The objective of this study was to evaluate the water sorption (Wsp) and ultimate tensile strength (UTS) of HEMA-containing/free one-step self-etch adhesives after long-term water-storage.

Methods

Three HEMA-containing one-step self-etch adhesives (Bond Force (BF), Clearfil S³ Bond (S3) and OptiBond All-In-One (OP)), and one HEMA-free one-step self-etch adhesive, G Bond (GB) was used. After the solvents of each adhesive were evaporated, polymerised adhesive disks and dumbbell-shaped specimens of thirty-two each were prepared and divided into four groups of 14-, 90-, 180- and 360-day water-storage. After immersion in water for the designated storage periods, the disks were subjected to measurement of Wsp, and the dumbbell-shaped specimens were subjected to measurement of UTS. The data of Wsp and UTS were statistically analysed using a two-way ANOVA and Bonferroni test.

Results

Wsp of BF, S3 and OP increased over time, whereas for GB, there were no significant differences in Wsp among all the storage periods. Wsp of GB was lower than those of BF, S3 and OP in each period. The UTS of BF, S3 and OP decreased over time, whereas for GB, there were no significant differences in UTS among all storage periods. The highest UTS was initially seen in BF > GB = S3 = OP, and after 360-day water-storage, seen in BF = GB > OP = S3.

Conclusions

For the HEMA-containing adhesives, Wsp increased and UTS decreased over time. On the other hand, for the HEMA-free adhesive, Wsp and UTS did not significantly change even after 360-day water-storage.     

自凝水凝胶义齿软衬材料吸水性与溶解性的实验研究

目的：研究自凝水凝胶义齿软衬材料的吸水性和溶解性。方法：自制的自凝水凝胶按应用比例调和制成直径50mm,厚1mm表面平整滑的圆片,干燥24h后称重（m1),再分别浸在人工唾液和蒸馏水溶液中保持7天和28天,称湿重（m2),继续干燥后称重（m3）,最后计算材料的吸水值、吸水性和溶解性,统计学分析处理。结果：水凝胶材料在人工唾液中7d和28d时的吸水率分别为28．62％和24．96％（P＜0．01）,溶解率分别为0．56％和0．51％（P＞0．05）;在蒸馏水中7d和28d时的吸水率分别为30．15％和27．85％（P＜0．01）,溶解率分别为0．79％和1．16％（P＜0．01）。结论随着浸泡时间的延长,水凝胶材料的吸水率呈下降的趋势,在蒸馏水中的材料吸水率和溶解率均分别高于同期在人工唾液中的吸水率和溶解率。作为一种义齿软衬材料,水凝胶可保持持续的柔软性,其临床效果还有待进一步研究。     

不同聚合方法对义齿基托树脂吸水性和溶解性的影响

目的 研究不同聚合方法对义齿基托树脂吸水性和溶解性的影响。方法 选择两种常用热凝义齿基托树脂材料,分别采用传统水浴法和电热聚合法制作样本,测量各样本的吸水值和溶解值。结果 日进水浴组、日进电热组、贺利氏水浴组、贺利氏电热组的吸水值依次为（25.48±3.04) μg/mm、（22.96±4.6) μg/mm、（22.65±5.44) μg/mm（18.21±5.19) μg/mm,以上各组的溶解值依次为（0.62±0.17) μg/mm、（0.54±0.18) μg/mm、（0.56±0.10) μg/mm、（0.51±0.11) μg/mm。日进水浴组的吸水值稍高,差别有统计学意义,其余各组比较均无差别。结论 不同聚合方法对义齿基托树脂吸水性和溶解性并无显著影响,所制作样本均符合国家标准。     

The influence of chemical structure on the properties in methacrylate-based dentin adhesives

Objectives

The objective of this study was to investigate the influence of the chemical structure of methacrylate monomers used in dentin adhesives on degree of conversion (DC), water sorption, and dynamic mechanical properties.

Materials and methods

Experimental adhesives containing 2,2-bis[4-(2-hydroxy-3-methacryloxypropoxy) phenyl]-propane (BisGMA), 2-hydroxyethyl methacrylate (HEMA), and co-monomer, 30/45/25 (w/w) were photo-polymerized. Ethyleneglycol dimethacrylate (EGDM), diethyleneglycol dimethacrylate (DEGDM), triethyleneglycol dimethacrylate (TEGDMA), 1,3-glycerol dimethacrylate (GDM), and glycerol trimethacrylate (GTM) were used as a co-monomer. The adhesives were characterized with regard to DC, water sorption, and dynamic mechanical analysis and compared to control adhesive [HEMA/BisGMA, 45/55 (w/w)].

Results

DC and water sorption increased with an increase in the number of ethylene glycol units in the monomer. Experimental adhesive containing GDM showed significantly higher storage moduli (p < 0.05) in both dry and wet samples than experimental adhesives containing EGDM or DEGDM. The rubbery moduli of adhesives containing GDM and GTM were found to be significantly greater (p < 0.05) than that of the control. Adhesives containing GTM exhibited the widest tan δ curves, indicating the greatest structural heterogeneity.

Significance

The hydrophilicity, functionality and size of monomers in dentin adhesives affected the water sorption, solubility, crosslink density and heterogeneity of the polymer network. The experimental adhesives containing GDM and GTM showed higher rubbery moduli, indicating higher crosslink density accompanied by a decrease in the homogeneity of the polymer network structure.     

Diffusion and concurrent solubility of self-adhering and new resin-matrix composites during water sorption/desorption cycles

Objectives

To investigate the kinetic process of water diffusion and mass change in new resin-matrix composites during water sorption/desorption cycles.

Methods

Five new resin-matrix composites were investigated [Filtek^® Silorane (FS), GC Gradia Direct Anterior (GDA), GC Gradia Direct Posterior (GDP), GC Kalore (GCK), Vertise^® Flow (VF)]. Five disk-shaped specimens, per material (15.0 ± 0.1) mm diameter by (2.0 ± 0.1) mm, were prepared according to ISO 4049. Each disk was immersed separately in de-ionized water for 150 d and then reconditioned for 75 d; all at (37 ± 1) °C. Mass was measured at different time intervals. Perspex disks were used as control. Data analysis was done by repeated measures ANOVA, one-way ANOVA and Tukey's post hoc test (p < 0.05).

Results

The water sorption (μg/mm³) after 150 d immersion ranged from 13.51 μg/mm³ (±0.40) for FS to 71.96 μg/mm³ (±0.90) for VF. The solubility ranged up to 16.95 μg/mm³ (±0.79) for VF. A significant mass reduction occurred in VF after the peak value [73.63 μg/mm³ (±0.31)] of water sorption was reached at 42 d. VF had the highest diffusion-coefficient for sorption: 5.23 × 10⁻⁹ cm²/s (±0.38) and desorption: 11.72 × 10⁻⁹ cm²/s (±0.16). Percentage sorption differences were significant for all materials (p < 0.001), except between GCK and GDP. The early correlation between mass change and square root of time was linear.

Significance

Each resin-matrix composite varied in sorption/desorption cycles which may affect clinical service. A concurrent solubility process occurred during sorption of the self-adhering composite VF. The silorane composite FS exhibited minimal sorption.     

Sorption of water, ethanol or ethanol/water solutions by light-cured dental dimethacrylate resins

Objectives

This work is concerned with the study of the sorption and desorption process of water, ethanol or ethanol/water solution 50% (v/v) or 75% (v/v) by the dental resins prepared by light curing of Bis-GMA, Bis-EMA, UDMA, TEGDMA or D₃MA.

Methods

A thin resin disc is placed in a bath of time to obtain the sorption curve m_t = f(t). Then the liquid is desorbed until a constant mass for the disc is reached and the desorption curve is recorded. These experimental curves help in the determination of the sorbed/desorbed liquid amount at equilibrium, the percentage of the extracted mass of unreacted monomer known as “solubility”, and the sorption/desorption diffusion coefficient which expresses correspondingly the rate of the liquid sorption/desorption.

Results

The highest liquid uptake by dental resins was 13.3 wt% ethanol for Bis-GMA-resin, 12.0 wt% ethanol for UDMA-resin, 10.10 wt% ethanol/water solution for TEGDMA-resin, 7.34 wt% ethanol for D₃MA-resin and 6.61 wt% ethanol for Bis-EMA-resin. The diffusion coefficient for all resins was higher in water than in ethanol/water solution or ethanol. Bis-GMA-resin showed the highest diffusion coefficient (11.01 × 10⁻⁸ cm² s⁻¹) followed by Bis-EMA-resin (7.43 × 10⁻⁸ cm² s⁻¹), UDMA-resin (6.88 × 10⁻⁸ cm² s⁻¹), D₃MA-resin (6.22 × 10⁻⁸ cm² s⁻¹) and finally by TEGDMA-resin (1.52 × 10⁻⁸ cm² s⁻¹).

Significance

All studied dental resins, except TEGDMA-resin, absorbed higher amount of pure ethanol than water or ethanol water solution. TEGDMA-resin absorbed higher amount of ethanol/water solution (50/50 or 75/25 (v/v)) than water or ethanol. For all studied dental resins the diffusion coefficient was higher in water than in ethanol/water solution or ethanol.     

氩等离子体对国产SY-1硅橡胶吸水率、溶解率的影响

目的：观察氩低温等离子体对国产SY-1硅橡胶吸水率、溶解率的影响。方法：将固化好的硅橡胶试样分组,按照不同工作参数组合对处理组SY-1硅橡胶试样进行氩气低温等离子体处理,处理后测定各组的吸水率、溶解率。结果：工作参数为1T,50W,1．5min时,材料吸水率降低显著;各参数下材料的溶解率未得到改善。结论：本实验条件下氩等离子体处理可以改善材料的吸水率,不能降低其溶解率。     

Water sorption and solubility of dental composites and identification of monomers released in an aqueous environment

Water sorption and solubility of six proprietary composite resin materials were assessed, and monomers eluted from the organic matrix during water storage identified. Water sorption and solubility tests were carried out with the following storage times: 4 h, 24 h and 7, 60 and 180 days. After storage, water sorption and solubility were determined. Eluted monomers were analysed by high performance liquid chromatography (HPLC). Correlation between the retention time of the registered peak and the reference peak was observed, and UV-spectra confirmed the identity. The results showed an increase in water sorption until equilibrium for all materials with one exception. The solubility behaviour of the composite resin materials tested revealed variations, with both mass decrease and increase. The resin composition influences the water sorption and solubility behaviour of composite resin materials. The HPLC analysis of eluted components revealed that triethyleneglycol dimethacrylate (TEGDMA) was the main monomer released. Maximal monomer concentration in the eluate was observed after 7 days. During the test period, quantifiable quantities of urethanedimethacrylate (UEDMA) monomer were observed, whereas 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)-phenyl]propane (Bis-GMA) was only found in detectable quantities. No detectable quantities of bisphenol-A were observed during the test period.     

10种复合树脂颜色稳定性与吸水溶解性研究

目的 评价10种光固化复合树脂在不同溶液中的颜色稳定性及吸水溶解性能。方法 10种光固化复合树脂分别为：BeautifilⅡ(B2)、Ceram. X One Universal (CXU)、Charisma (CS)、Charisma Diamond (CD)、Denfil (DF)、DX. Universal (DXU)、Filtek Z250 (Z250)、Filtek Z350 XT (Z350)、FS-1 (FS)、Magnafill Putty(MP)。每种树脂材料各制作20个试件,随机分为4组(n=5),分别浸入蒸馏水(对照组)、咖喱、咖啡和红酒28 d,分光光度计测量试件浸入前及浸入后1、7、14、21和28 d的色度值(CIE L^*a^*b^*),计算染色前后色差值。根据ISO 4049:2019标准,每种材料制作3个试件,测量材料的吸水性和溶解性。采用三因素方差分析评估树脂材料、染液、染色时间对染色前后色差值(ΔE)的影响,采用单因素方差分析比较不同材料的吸水值和溶解值变化。结果 随着染色时间增加,所有试...     

Sealing ability, water sorption, solubility and toothbrushing abrasion resistance of temporary filling materials

Aim To evaluate marginal seal, water sorption, solubility and loss of mass after brushing of several temporary filling materials. Methodology For marginal seal, Class I cavities, including endodontic access preparations, were made in human molar teeth and restored using one or other of several temporary filling materials (n = 10): zinc oxide/calcium sulphate‐based cement (Cavit, 3M,ESPE, St. Paul, MN, USA), zinc oxide/eugenol cement (IRM, Dentsply Caulk, Milford, DE, USA), glass ionomer cement (Vidrion R, SSWhite, Rio de Janeiro, RJ, Brazil) or a dimethacrylate‐based filling (Bioplic, Biodinâmica, Londrina, PR, Brazil). Dye penetration was assessed after thermocycling and immersion in 0.5% basic fuchsine solution. For water sorption, solubility and loss of mass analyses, disc‐shaped specimens were made. Water sorption and solubility were evaluated by mass alteration after storage in distilled water for 7 days (n = 7). Loss of mass was calculated based on the difference of mass after abrasion with a toothbrush (n = 5), and surfaces were analysed by SEM. Data of water sorption, solubility and loss of mass were submitted to anova and Tukey’s test, and marginal sealing data to Kruskal–Wallis test (P < 0.05). Results Statistically significant differences were observed for marginal sealing (P < 0.0001), water sorption (P < 0.01), solubility (P < 0.01) and loss of mass (P < 0.05). Bioplic had the best marginal seal. Cavit had the greatest water sorption and solubility. Vidrion R and Bioplic had the lowest solubility. Loss of mass after brushing was higher for Cavit, followed by Bioplic, IRM and Vidrion R. Cavit and Vidrion R were worn aggressively by brushing. Conclusions The resin‐based temporary filling Bioplic produced the best marginal seal, and was associated with the lowest water sorption, solubility and loss of mass.     

三种颌面赝复硅橡胶吸水率、溶解率的对比测定

目的:对比研究ZY-1、SY-1及A-2186三种赝复硅橡胶的吸水率和溶解率,评价ZY-1硅橡胶的对水的稳定性.方法:在相同条件下对三种硅橡胶材料进行吸水率和溶解率测定,并对结果进行统计学分析.结果:ZY-1的吸水率及溶解率与A-2186无显著性差异,而明显低于SY-1.结论:赝复硅橡胶材料ZY-1具有良好的水解稳定性.     

SY-1及MDX4-4210硅橡胶吸水率溶解率撕裂强度的对比测定

目的：对比SY－1和MDX4－4210硅橡胶的吸水率，溶解率，撕裂强度性能。方法：在相同条件下对两种硅橡胶材料进行吸水率，溶解率及撕裂强度测定，对其进行t检验分析。结果：SY－1硅橡胶吸水率，溶解率性能差于MDX4－4210硅橡胶，撕裂强度优于MDX4－4210硅橡胶。结论：SY－1硅橡胶的撕裂强度符合作为颌面部软组织缺损的赝复材料要求；作为与液体有密切接触的赝复材料时，其吸水率，溶解率性能尚须进一步改进。     

Chlorhexidine release and water sorption characteristics of chlorhexidine-incorporated hydrophobic/hydrophilic resins

OBJECTIVES: The aim of this study was to evaluate chlorhexidine release from unfilled non-solvated methacrylate-based resins of increasing hydrophilicity and to examine relationships among Hoy's solubility parameters, water sorption, solubility and the rate of chlorhexidine release. METHODS: Resin discs were prepared from light-cured, experimental resin blends (R1, R2, R3, R4 and R5) containing 0.0, 0.2, 1.0 and 2.0wt.% chlorhexidine diacetate (CDA). Discs were immersed in distilled water at 37 degrees C, and mass changes were recorded at different periods. Spectral measurements were made to follow change in optical densities of storage solution to examine chlorhexidine release kinetics. After a 28-day period, water sorption, solubility, and the cumulative chlorhexidine release were obtained. Additionally, antibacterial study was performed by observing the presence of inhibition zone against Streptococcus mutans. RESULTS: The most hydrophilic resin (R5) exhibited the highest chlorhexidine release rate. The most hydrophobic resin (R1) exhibited the lowest rate. However, no inhibition zone was produced by any specimens stored in water for 2 weeks. The addition of CDA increased solubility significantly but had no effect on water sorption. Significant positive correlations were seen between water sorption and the cumulative chlorhexidine release. SIGNIFICANCE: Chlorhexidine release from resins may be related to water-induced swelling, which in turn is enhanced by the hydrophilicity of cured polymer matrix.     

四氟甲烷等离子体对赝复硅橡胶吸水率、溶解率影响

目的：观察四氟甲烷（CF4）低温等离子体对两种赝复硅橡胶吸水率、溶解率的影响。方法：将固化好的硅橡胶试样分组,按照不同工作参数组合对处理组赝复硅橡胶试样进行CF4低温等离子体处理,处理后测定各组的吸水率、溶解率。结果：对于两种硅橡胶,均可以找到降低吸水率的CF4低温等离子体处理工作参数组合,而均未找到降低溶解率的工作参数组合。结论：本实验条件下应用CF4等离子体表面处理技术,可以有效地降低两种赝复用硅橡胶的吸水率,但是不能有效地降低两种硅橡胶的溶解率,需寻求其他方法解决。     

Effect of ozone gas application on the mechanical properties of dental adhesives bonded to dentin

OBJECTIVES: To assess the effect of ozone gas on the mechanical properties of different classes of dental adhesives. METHODS: Extracted molars were sectioned perpendicularly to their long axis for obtaining dentin slices to be bonded with one of the following adhesives: Prime&Bond NT (Dentsply), Excite (Ivoclar-Vivadent), Syntac/Heliobond (Ivoclar-Vivadent) and Silorane System Adhesive (3M-ESPE). Prior to bonding, the slices were sectioned in two halves: one was treated with ozone gas for 120s (4.2g/m(3); HealOzone, KaVo) and the other served as control. The Vicker's hardness (VH), elastic modulus (E), elastic work (W(e)/W(tot)) and the creep (Cr) of the materials were measured with an automatic micro hardness indenter (Fischer) 30min and 24h after bonding procedure. Data were analyzed with the multivariate ANOVA followed by the Tukey's test and partial eta-squared statistics. RESULTS: The adhesive and the time of testing were significant factors affecting the investigated parameters (p<0.001; eta(p)(2)>/=0.06). Dentin treatment, though significant, exerted a minimal effect on mechanical properties (eta(p)(2)相似文献