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Microleakage of various cementing agents for full cast crowns

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Dental Materials (2005) 21, 445–453<br />

<strong>Microleakage</strong> <strong>of</strong> <strong>various</strong> <strong>cementing</strong> <strong>agents</strong><br />

<strong>for</strong> <strong>full</strong> <strong>cast</strong> <strong>crowns</strong><br />

Andree Piwowarczyk a, *, Hans-Christoph Lauer a , John A. Sorensen b<br />

a<br />

Department <strong>of</strong> Prosthetic Dentistry, School <strong>of</strong> Dentistry, Johann Wolfgang Goethe University,<br />

Theodor-Stern-Kai 7, 60590 Frankfurt, Germany<br />

b<br />

Pacific Dental Institute, Portland, OR, USA<br />

Received 5 November 2003; received in revised <strong>for</strong>m 1 June 2004; accepted 13 July 2004<br />

KEYWORDS<br />

Cementing agent;<br />

<strong>Microleakage</strong>;<br />

Marginal gap;<br />

Full <strong>cast</strong> <strong>crowns</strong><br />

* Corresponding author. Tel.: C49 69 6301 5640; fax: C49 69<br />

6301 3711.<br />

E-mail address: piwowarczyk@t-online.de (A. Piwowarczyk).<br />

Summary Objectives. To evaluate microleakage and marginal gaps in <strong>full</strong> <strong>cast</strong><br />

crown restorations bonded with six different types <strong>of</strong> <strong>cementing</strong> <strong>agents</strong>.<br />

Methods. Sixty non-carious human premolars and molars were prepared in a<br />

standardized manner <strong>for</strong> <strong>full</strong> <strong>cast</strong> crown restorations. The mesial and distal margins<br />

were located in dentin, while the vestibular and palatal/lingual margins were located<br />

in enamel. Crowns were made from a high-gold alloy using a standardized technique.<br />

The specimens were randomized to six groups <strong>of</strong> <strong>cementing</strong> <strong>agents</strong>: one zincphosphate<br />

cement (Harvard cement), one conventional glass–ionomer cement (Fuji<br />

I), one resin-modified glass–ionomer cement (Fuji Plus), two standard resin cements<br />

(RelyX ARC, Panavia F), and one self-adhesive universal resin cement (RelyX<br />

Unicem). After 4 weeks <strong>of</strong> storage in distilled water at 37 8C, the specimens were<br />

subjected to 5000 thermocycles ranging from 5 to 55 8C. Then, they were placed in a<br />

silver nitrate solution, embedded in resin blocks, and vertically cut in buccolingual<br />

and mesiodistal direction. Subsequently, the objects were evaluated <strong>for</strong> microleakage<br />

and marginal gap using a high-resolution digital microscope camera.<br />

Results. A number <strong>of</strong> inter-group differences were statistically significant. RelyX<br />

Unicem showed the smallest degree <strong>of</strong> microleakage both in enamel and in dentin.<br />

Panavia F und RelyX Unicem were associated with significantly larger marginal gaps<br />

than all other <strong>cementing</strong> <strong>agents</strong>. No association was observed between microleakage<br />

and marginal gap other than a weak direct correlation when using Harvard cement on<br />

enamel.<br />

Significance. The <strong>cementing</strong> <strong>agents</strong> investigated revealed different sealing<br />

abilities. These differences were not associated with specific types <strong>of</strong> materials.<br />

Q 2004 Academy <strong>of</strong> Dental Materials. Published by Elsevier Ltd. All rights reserved.<br />

Introduction<br />

www.intl.elsevierhealth.com/journals/dema<br />

In vitro studies <strong>of</strong> microleakage are an initial<br />

screening method to assess the maximum theoretical<br />

loss <strong>of</strong> sealing ability in vivo [1]. The occurrence<br />

<strong>of</strong> microleakage along the interface has been<br />

0109-5641/$ - see front matter Q 2004 Academy <strong>of</strong> Dental Materials. Published by Elsevier Ltd. All rights reserved.<br />

doi:10.1016/j.dental.2004.07.009


446<br />

related to pulpal problems [2,3], hypersensitivity,<br />

and secondary caries [4], the latter being the most<br />

common reason why restorations are replaced [5].<br />

Few studies have dealt with microleakage in <strong>full</strong><br />

<strong>cast</strong> <strong>crowns</strong> based on different types <strong>of</strong> <strong>cementing</strong><br />

<strong>agents</strong> [6–10]. Moreover, the methodologies and<br />

<strong>cementing</strong> <strong>agents</strong> used in these studies have been<br />

too diverse to allow direct comparison <strong>of</strong> the data.<br />

But it is possible to analyze different types <strong>of</strong><br />

commercially available <strong>cementing</strong> <strong>agents</strong> that can<br />

be used <strong>for</strong> long-term cementation <strong>of</strong> fixed restorations.<br />

These include zinc-phosphate cements,<br />

conventional glass–ionomer cements, resin-modified<br />

glass–ionomer cements, standard resin<br />

cements, and a recently developed material<br />

described as self-adhesive universal resin cement.<br />

The objective in developing this cement was to<br />

combine the ease <strong>of</strong> handling <strong>of</strong>fered by glass–<br />

ionomer cements with the favorable mechanical<br />

properties [11], attractive esthetics [12], and good<br />

adhesion <strong>of</strong> resin cements [13].<br />

A review <strong>of</strong> the literature by Raskin et al. [14]<br />

showed that 62.5% out <strong>of</strong> 144 studies on microleakage<br />

per<strong>for</strong>med between 1992 and 1998 evaluated<br />

microleakage in Class V cavities, while only<br />

4.3% evaluated microleakage and marginal gaps as<br />

study parameters involved in crown restorations.<br />

These latter include only a limited number <strong>of</strong><br />

studies [9,10] investigating the correlation between<br />

microleakage and marginal gaps in <strong>full</strong> <strong>cast</strong> <strong>crowns</strong>;<br />

no such correlation was found. However, the<br />

significance <strong>of</strong> the marginal gaps <strong>of</strong> <strong>full</strong> <strong>cast</strong><br />

restorations and their clinical consequences remain<br />

to be determined.<br />

The objective <strong>of</strong> the present in vitro study was to<br />

investigate microleakage and marginal gaps associated<br />

with <strong>cementing</strong> <strong>agents</strong> in <strong>full</strong> <strong>cast</strong> <strong>crowns</strong><br />

following artificial aging. Other questions to be<br />

examined were (1) whether <strong>various</strong> types <strong>of</strong><br />

<strong>cementing</strong> <strong>agents</strong> produce the same sealing ability<br />

<strong>for</strong> definite bonding <strong>of</strong> indirect restorations and (2)<br />

in how far microleakage results differ depending on<br />

whether the margins <strong>of</strong> the restoration are placed in<br />

dentin or in enamel. A final objective was to<br />

determine whether there was a connection between<br />

microleakage and marginal gaps in <strong>full</strong> <strong>cast</strong> <strong>crowns</strong>.<br />

Materials and Methods<br />

Specimen preparation<br />

A total <strong>of</strong> 60 freshly extracted non-carious permanent<br />

human molars with <strong>full</strong>y developed roots were<br />

selected <strong>for</strong> this study. All teeth were stored in<br />

A. Piwowarczyk et al.<br />

distilled water at room temperature immediately<br />

after extraction. Calculus and residual periodontal<br />

tissue were removed using a surgical knife, scaler,<br />

and curette. Subsequently, the teeth were conservatively<br />

polished using a rotating brush and<br />

pumice.<br />

The preparations <strong>for</strong> the <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> were<br />

per<strong>for</strong>med using a suitable design and a converging<br />

angle <strong>of</strong> around 68 to achieve optimal retention and<br />

resistance properties. The occlusal and axial surfaces<br />

were reduced by approximately 1.2 and<br />

0.8 mm, respectively. The cervical preparation<br />

margins were designed as circular chamfers using<br />

torpedo-shaped diamond burs and water-cooling<br />

(Gebr. Brasseler, Lemgo, Germany; No. 878,314,<br />

size 012). The preparations were finished with the<br />

help <strong>of</strong> magnifying loupes (magnification !3.5;<br />

Zeiss, Oberkochen, Deutschland; serial #53-20)<br />

using fine and extra-fine diamond burs (Gebr.<br />

Brasseler, Lemgo, Germany; No. 8878.314 and<br />

878EF.314, size 012). Subsequently, a final check<br />

<strong>of</strong> the preparations was per<strong>for</strong>med. The mesial and<br />

distal margins were located in dentin, while the<br />

vestibular and palatal/lingual margins were located<br />

in enamel.<br />

For the model dies, impressions <strong>of</strong> the prepared<br />

teeth were taken with Impregum Penta (3M ESPE,<br />

Seefeld, Germany) and poured with Type IV resinstabilized<br />

extra-hard stone (esthetic-base 300;<br />

dentona AG, Dortmund, Germany; lot #51001742)<br />

following the manufacturer’s mixing instructions.<br />

The stone was allowed to set <strong>for</strong> 40 min and then<br />

removed from the impression. The resultant stone<br />

dies were trimmed and covered with stone hardener<br />

(Classic Hardener Spacer clear; Kerr Lab, Belle<br />

de St Claire, France) followed by two layers <strong>of</strong> die<br />

spacer (Classic Cement Spacer blue; Kerr Lab, Belle<br />

de St Claire, France) above the preparation margin.<br />

The preparation margin was marked with a nongraphite<br />

pencil under a stereomicroscope at !32<br />

magnification (Zeiss, Oberkochen, Germany; Stemi<br />

2000-C, serial #2004003753). Subsequently, red<br />

cervical wax and blue modeling wax (YETI Dentalprodukte,<br />

Engen, Germany) were used to model <strong>full</strong><br />

<strong>crowns</strong> <strong>of</strong> 0.5 mm thickness. Four round reference<br />

marks approximately 1.5 mm in diameter were<br />

applied in the mesial, distal, vestibular and<br />

lingual/palatal segments centrally around 3 mm<br />

above the preparations located in enamel and<br />

dentin. Five wax copings each were embedded in<br />

a #3 muffle ring with phosphate-bonded investment<br />

(Precibalite plus; Dentona AG, Dortmund,<br />

Germany; lot #0501101). After setting, the muffle<br />

was heated and a centifugal <strong>cast</strong>ing per<strong>for</strong>med<br />

using a Type IV high-gold <strong>cast</strong>ing alloy (Portadur P4;<br />

Wieland Edelmetalle GmbH, P<strong>for</strong>zheim, Germany;


<strong>Microleakage</strong> <strong>of</strong> <strong>various</strong> <strong>cementing</strong> <strong>agents</strong> <strong>for</strong> <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> 447<br />

relative constituents: Au 68.5%, Ag 12.0%, Cu 12.0%,<br />

Pt 6.9%, Zn 0.5%, Ir 0.1%; lots #4492 and 4269).<br />

The <strong>cast</strong>ings were divested, trimmed and seated<br />

using well-established procedures routinely used by<br />

dental laboratories <strong>for</strong> crown restorations. The fit<br />

<strong>of</strong> the <strong>cast</strong>ings was checked with silicone (Fit<br />

Checker; GC, Munich, Germany) and improved if<br />

necessary. Any points visibly pressed into the<br />

silicone were relieved using a small (0.08 mm in<br />

diameter) rotary instrument. The marginal fit <strong>of</strong> all<br />

<strong>cast</strong>ings was verified on the prepared residual teeth<br />

under a stereomicroscope (!32 magnification) and<br />

with an extra-fine probe (EXD5; Hu-Friedy, Chicago,<br />

IL, USA). Subsequently, the interior surface <strong>of</strong> the<br />

gold frameworks was sandblasted with Al 2O 3<br />

(Hasenfratz, Grafing, Germany; average grain<br />

size, 105 mm; pressure, 0.18 MPa; distance,<br />

10 mm; duration, 10 s).<br />

Our experimental set-up included one zincphosphate<br />

cement (Harvard cement), one conventional<br />

glass–ionomer cement (Fuji I), one resinmodified<br />

glass–ionomer cement (Fuji Plus), two<br />

standard dual-cure resin cements (RelyX ARC,<br />

Panavia F), and one recently developed dualcure<br />

self-adhesive resin cement (RelyX Unicem)<br />

(Table 1). All <strong>cementing</strong> <strong>agents</strong> were processed<br />

at room temperature (23 8C) strictly following<br />

the manufacturers’ instructions. Two cements<br />

(GC Fuji Plus and RelyX Unicem) were supplied<br />

in pre-measured capsules. Upon activation, these<br />

materials were mechanically triturated with the<br />

rotational mixing machine (CapMix; 3M ESPE,<br />

Seefeld, Germany) <strong>for</strong> the time recommended by<br />

the manufacturers (10 or 15 s). RelyX ARC was<br />

supplied in pre-measured delivery systems. Panavia<br />

F was mixed on a mixing block, using a hard<br />

plastic spatula, at a base-to-catalyst paste ratio <strong>of</strong><br />

1:1 <strong>for</strong> approximately 20 s. An oxygen-blocking gel<br />

(Oxyguard II; Kuraray, Osaka, Japan; lot #00373A)<br />

was applied <strong>for</strong> 3 min when Panavia F was used.<br />

Fuji I was manually mixed at a powder-to-liquid<br />

ratio <strong>of</strong> 1.8–1.0 <strong>for</strong> around 20 s. The powder-toliquid<br />

ratio <strong>of</strong> Harvard cement was determined by<br />

weighing according to the manufacturer’s instructions<br />

using an analytical balance (G1 mg). Mixing<br />

was per<strong>for</strong>med on a cool slab, over a wide area,<br />

to incorporate small increments <strong>of</strong> powder into<br />

the liquid <strong>for</strong> approximately 90 s (Harvard<br />

cement).<br />

Be<strong>for</strong>e cementation, all 60 teeth were randomized<br />

along with their gold frameworks to six test<br />

groups (nZ10). The interior surfaces <strong>of</strong> the crown<br />

restorations and the prepared teeth were cleaned<br />

with alcohol. All teeth, which were to receive the<br />

resin-modified glass–ionomer cement or a standard<br />

resin cement, were pretreated with dentin<br />

Table 1 Description <strong>of</strong> <strong>cementing</strong> <strong>agents</strong> used in this study.<br />

Materials Type Main composition a<br />

Adhesive system Manufacturer<br />

Harvard cement Zinc-phosphate P: zinc oxide, magnesia; No adhesive system Richter & H<strong>of</strong>fmann,<br />

(Batch No. powder<br />

2112498001, Batch<br />

No. liquid<br />

2111000013)<br />

cement<br />

L: phosphoric acid<br />

Berlin, Germany<br />

Fuji I (Batch No. Conventional P: polyacrylic acid, alu- No adhesive system GC Corp., Tokyo,<br />

0001251)<br />

glass–ionomer mino-silicate glass;<br />

Japan<br />

cement<br />

L: polyacrylic acid,<br />

citric acid<br />

Fuji Plus (Batch No. Resin-modified P: alumino-silicate Fuji Plus conditioner GC Corp., Tokyo,<br />

0009214)<br />

glass–ionomer glass; L: HEMA, poly-<br />

Japan<br />

cement<br />

acrylic acid, TEGDMA<br />

RelyX ARC (Batch No. Resin cement Bis-GMA, TEGDMA, silica Single bond adhesive 3M ESPE, Seefeld,<br />

CACA)<br />

and zirconium glass (Batch No. 4242) Germany<br />

Panavia F (Batch No. Resin cement BPEDMA, MDP, DMA, ED primer (Batch No. Kuraray, Osaka,<br />

base 00124A, Batch<br />

barium, boron and sili- 00108B, Batch No. Japan<br />

No. catalyst 00046A)<br />

cium glass, NaF<br />

00115B)<br />

RelyX Unicem (Batch Self-adhesive Phosphoric acid metha- No adhesive system 3M ESPE, Seefeld,<br />

No. 0001)<br />

universal resin crylates,dimethacry- Germany<br />

cement<br />

lates, inorganic fillers,<br />

fumed silica, initiators<br />

P, powder; L, liquid. Bis-GMA, bisphenol-A diglycidyl ether dimethacrylate; BPEDMA, bisphenol-A polyethoxydimethacrylate; DMA,<br />

aliphatic dimethacrlyate; HEMA, 2-hydroxyethylmethacrylat; MDP, 10-methacryloyloxy decyl dihydrogenphosphate; NaF, sodium<br />

fluoride; TEGDMA, triethylene glycol dimethacrylate.<br />

a According to the in<strong>for</strong>mation provided by the manufacturers.


448<br />

adhesives as recommended by the manufacturers<br />

(Table 1). Dentin adhesives were not used <strong>for</strong> the<br />

zinc-phosphate cement, the conventional glass–<br />

ionomer cement, and the self-adhesive resin<br />

cement. Bonding was per<strong>for</strong>med by loading the<br />

<strong>cementing</strong> agent into the interior surface <strong>of</strong> the<br />

restoration and applying finger pressure <strong>for</strong> 10 s.<br />

Then the frameworks were axially loaded at a<br />

constant weight <strong>of</strong> 58.8 N <strong>for</strong> 7 min [15]. Excess<br />

cement was removed with a scaler; marginal fit was<br />

checked both by visual inspection and with a probe.<br />

All tooth-restoration specimens were stored in<br />

distilled water at 37 8C <strong>for</strong> 4 weeks, then they were<br />

subjected to 5000 thermocycles ranging from 5 to<br />

55 8C (immersion time, 20 s; transfer time, 10 s).<br />

Subsequently, the root surfaces <strong>of</strong> the restored<br />

teeth were covered with two layers <strong>of</strong> nail varnish<br />

(ending 2 mm below the crown margin) and subjected<br />

to silver nitrate penetration [16]. Then<br />

they were placed into an unimolar silver nitrate<br />

solution (Crystal, Fisher Scientific, Fairfield, NJ,<br />

USA) <strong>for</strong> 6 h, followed by thorough rinsing, storage<br />

in a photochemical developer (Solutek Corporation,<br />

Boston, MA, USA) <strong>for</strong> 12 h, and exposure to a 150-W<br />

floodlamp <strong>for</strong> 6 h.<br />

Next, the tooth-restoration specimens were<br />

embedded in a transparent resin matrix (Buehler<br />

Epoxide; Buehler, Lake Bluff, IL, USA), which was<br />

allowed to harden at room temperature <strong>for</strong> 24 h.<br />

Each resin block was cut twice in the buccolingual<br />

and the mesiodistal direction along the previously<br />

applied reference marks using a slow-speed diamond<br />

saw (Isomet; Buehler Ltd, Evanston, IL, USA) with<br />

water-cooling. In this way, each specimen featured<br />

eight surfaces (four in enamel and four in dentin) <strong>for</strong><br />

analysis <strong>of</strong> microleakage and marginal gap. The cut<br />

surfaces were once again placed under a 150-W<br />

floodlamp <strong>for</strong> 5 min, such that all portions <strong>of</strong> the<br />

silver nitrate penetration acquired a black color.<br />

Evaluation <strong>of</strong> microleakage and marginal gap<br />

using a high-resolution digital microscope<br />

camera<br />

The microleakage in the area <strong>of</strong> the tooth–cement<br />

interface was defined as linear penetration <strong>of</strong> silver<br />

nitrate starting from the restorative crown margins<br />

[17] and was determined with a stereomicroscope<br />

(475052-9901; Zeiss, Oberkochen, Germany) and<br />

AxioCam HR digital microscope camera (Zeiss,<br />

Oberkochen, Germany; s<strong>of</strong>tware module: Axio<br />

Vision 3.1). The images were taken at a resolution<br />

<strong>of</strong> 1300!1030 pixels. A micrometer scale (474026;<br />

Zeiss, Oberkochen, Germany) was placed diagonally<br />

across the image <strong>for</strong> calibration. The maximum<br />

potential calibration-related error due to the width<br />

<strong>of</strong> mapped lines was G0.709 or G0.475% depending<br />

on the magnification factor relative to the absolute<br />

measured values. Depending on the magnification,<br />

2.42 or 3.64 mm/pixel were obtained. Metric assessment<br />

<strong>of</strong> distances was per<strong>for</strong>med using micrometers<br />

(mm) as units. A randomly selected image including<br />

10 measurements was analyzed to determine the<br />

potential mapping error due to the definition <strong>of</strong><br />

microleakage length. Given a measured length <strong>of</strong><br />

1 mm, a maximum mapping error <strong>of</strong> G0.01 mm was<br />

obtained irrespective <strong>of</strong> the magnification factor.<br />

Marginal gaps were measured as defined by<br />

Holmes et al. [18] using the stereomicroscope<br />

(4730129901; Zeiss, Oberkochen, Germany) and<br />

digital microscope camera. The selected magnification<br />

was based on 1.21 mm equaling one pixel.<br />

Based on the absolute values measured, the<br />

maximum calibration-related error was G0.154%.<br />

A randomly selected image including 10 measurements<br />

was analyzed to determine the potential<br />

mapping error due to the definition <strong>of</strong> marginal gap<br />

length. Given a length <strong>of</strong> 40 mm, a maximum<br />

mapping error <strong>of</strong> G0.18 mm was obtained.<br />

Statistical analysis<br />

Descriptive representation <strong>of</strong> continuous variables<br />

was based on mean values, SD, and minimum–<br />

maximum values. In addition, a number <strong>of</strong> tests<br />

(skewness test, kurtosis test, and omnibus test)<br />

were used to analyze whether the frequency<br />

distribution <strong>of</strong> the random sample differed significantly<br />

from the normal distribution. Since, the bulk<br />

<strong>of</strong> data was not characterized by a normal<br />

distribution, a non-parametric Kruskal–Wallis test<br />

was used to analyze differences in the <strong>various</strong><br />

groups <strong>of</strong> <strong>cementing</strong> <strong>agents</strong>, comparing the<br />

obtained test parameters (Bonferroni-corrected p<br />

values). A non-parametric Wilcoxon’s test was used<br />

to evaluate the differences between enamel and<br />

dentinal substrates. The selected level <strong>of</strong> statistical<br />

significance was p!0.05. Spearman’s correlation<br />

coefficient (R) was used to assess the correlation<br />

between two continuous variables.<br />

Results<br />

A. Piwowarczyk et al.<br />

<strong>Microleakage</strong> with preparation margins<br />

in enamel<br />

Fig. 1 illustrates the mean values and SD <strong>for</strong> the<br />

microleakage findings obtained with the <strong>various</strong><br />

<strong>cementing</strong> <strong>agents</strong>. The smallest degree <strong>of</strong>


<strong>Microleakage</strong> <strong>of</strong> <strong>various</strong> <strong>cementing</strong> <strong>agents</strong> <strong>for</strong> <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> 449<br />

Figure 1 Mean values and SD <strong>for</strong> microleakage, based<br />

on 40 measurements <strong>for</strong> each material, with preparation<br />

margins located in enamel.<br />

microleakage was observed with the dual-cure selfadhesive<br />

resin cement (RelyX Unicem; 0.70G<br />

0.61 mm), followed by the conventional glass–<br />

ionomer cement (Fuji I; 0.71G0.32 mm), and the<br />

resin-modified glass–ionomer cement (Fuji Plus;<br />

0.77G0.48 mm). The greatest degree <strong>of</strong> microleakage<br />

was observed with the zinc-phosphate (Harvard)<br />

cement (1.59G0.64 mm). The Kruskal–Wallis<br />

test revealed statistically significant differences<br />

between the zinc-phosphate (Harvard) cement on<br />

one hand and all other <strong>agents</strong> (all p!0.01) with the<br />

exception <strong>of</strong> standard resin cement (RelyX ARC) on<br />

the other. A significant difference was also established<br />

between one standard resin cement (RelyX<br />

ARC) and the self-adhesive resin cement (RelyX<br />

Unicem) (pZ0.019).<br />

<strong>Microleakage</strong> with preparation margins in<br />

dentin<br />

Fig. 2 illustrates the microleakage findings with<br />

preparation margins located in dentin. The smallest<br />

degree <strong>of</strong> microleakage was observed with<br />

the self-adhesive resin cement (RelyX Unicem;<br />

1.01G0.54 mm), followed by the resin-modified<br />

glass–ionomer cement (Fuji Plus; 1.39G0.49 mm),<br />

and the conventional glass–ionomer cement (Fuji<br />

I; 1.41G0.90 mm). Statistically significant differences<br />

were observed between the zinc-phosphate<br />

(Harvard) cement and both the conventional glass–<br />

ionomer cement (Fuji I, pZ0.006) and the selfadhesive<br />

resin cement (RelyX Unicem, p!0.0001),<br />

between the conventional glass–ionomer cement<br />

(Fuji I) and the standard resin cement (RelyX ARC,<br />

pZ0.002), between the resin-modified glass–ionomer<br />

cement Fuji Plus and the standard<br />

resin cement RelyX ARC (pZ0.0281), between<br />

Figure 2 Mean values and SD <strong>for</strong> microleakage, based<br />

on 40 measurements <strong>for</strong> each material, with preparation<br />

margins located in dentin.<br />

the standard resin cement RelyX ARC and the selfadhesive<br />

resin cement RelyX Unicem (p!0.0001),<br />

and between the standard resin cement Panavia F<br />

and the self-adhesive resin cement RelyX Unicem<br />

(p!0.0001).<br />

<strong>Microleakage</strong> with preparation margins in<br />

enamel versus dentin<br />

All test groups revealed significant differences in<br />

microleakage between enamel and dentin. <strong>Microleakage</strong><br />

was invariably more pronounced in dentin<br />

than in enamel (Table 2).<br />

Marginal gap<br />

The average marginal gap in the specimens ranged<br />

from 47.70G17.92 mm <strong>for</strong> the zinc-phosphate<br />

(Harvard) cement up to 74.59G29.15 mm <strong>for</strong> the<br />

self-adhesive resin cement (RelyX Unicem; Fig. 3).<br />

The difference between one <strong>of</strong> the standard resin<br />

Table 2 Comparative microleakage data (mean<br />

values and SD) with preparation margins in enamel or<br />

dentin.<br />

Enamel<br />

(mm)<br />

Dentin<br />

(mm)<br />

p value<br />

Harvard<br />

cement<br />

1.59 (0.64) 2.01 (0.70) 0.0054<br />

Fuji I 0.71 (0.32) 1.41 (0.90) 0.000003<br />

Fuji Plus 0.77 (0.48) 1.39 (0.49) 0.000008<br />

RelyX ARC 1.11 (0.68) 2.19 (1.04) 0.0000001<br />

Panavia F 0.95 (0.59) 2.11 (1.35) 0.000001<br />

RelyX Unicem 0.70 (0.61) 1.01 (0.54) 0.0098<br />

Inter-group differences were evaluated by Wilcoxon’s test<br />

and were statistically significant in all groups (p!0.05).


450<br />

Figure 3 Mean values and SD <strong>for</strong> marginal gap based on<br />

80 measurements <strong>for</strong> each material.<br />

cements (Panavia F) and the self-adhesive resin<br />

cement (RelyX Unicem) was not statistically significant.<br />

Both, however, differed significantly from all<br />

other <strong>cementing</strong> <strong>agents</strong> (all p!0.01).<br />

Correlation between microleakage<br />

and marginal gap<br />

A weak direct correlation between microleakage<br />

and marginal gap was observed in the enamel <strong>of</strong><br />

specimens in which the zinc-phosphate cement<br />

(Harvard) had been used <strong>for</strong> bonding (correlation<br />

coefficient, RZ0.41). No such correlation was<br />

found in any <strong>of</strong> the other groups.<br />

Discussion<br />

It is well established that the type <strong>of</strong> <strong>cementing</strong><br />

agent used <strong>for</strong> bonding has a bearing on microleakage<br />

[17,19]. It is also known that the composition<br />

and other special characteristics <strong>of</strong> <strong>cementing</strong><br />

<strong>agents</strong> (e.g. the setting properties and the dentin<br />

adhesive used) determine the degree <strong>of</strong> leakage.<br />

The smallest degree <strong>of</strong> microleakage, both in<br />

enamel and in dentin, was obtained with the selfadhesive<br />

resin cement (RelyX Unicem). Apparently,<br />

there<strong>for</strong>e, this agent is capable <strong>of</strong> generating an<br />

effective seal at the interfaces between restorative<br />

alloy, <strong>cementing</strong> agent, and dental tissue without<br />

requiring pretreatment <strong>of</strong> the prepared tooth<br />

surfaces. The <strong>for</strong>mulation <strong>of</strong> RelyX Unicem contains<br />

specific multifunctional phosphoric-acid methacrylates<br />

able to interact with the tooth surface in<br />

multiple ways, such as by <strong>for</strong>ming complex compounds<br />

with calcium ions or by different kinds<br />

<strong>of</strong> physical interaction like hydrogen bonding or<br />

dipole-to-dipole interactions. This variety <strong>of</strong> interactions<br />

seems to enable RelyX Unicem to generate<br />

A. Piwowarczyk et al.<br />

self-adhesion to both enamel and dentin, resulting<br />

in an effective seal <strong>of</strong> the tooth–cement interface<br />

and hence in the lowest microleakage values in<br />

enamel and dentin <strong>of</strong> all luting <strong>agents</strong> examined.<br />

The two standard dual-cure resin cements (RelyX<br />

ARC and Panavia F) were associated with a higher<br />

degree <strong>of</strong> microleakage—both in enamel and in<br />

dentin—than the conventional glass–ionomer<br />

cement (Fuji I) and the resin-modified glass–<br />

ionomer cement (Fuji Plus). In general, different<br />

microleakage patterns may be caused by different<br />

factors, depending on the type <strong>of</strong> <strong>cementing</strong> agent<br />

used and the experimental conditions.<br />

The greater leakage <strong>of</strong> the resin cements RelyX<br />

ARC and Panavia F compared to the conventional<br />

glass–ionomer cement Fuji I and the resin-modified<br />

glass–ionomer Fuji Plus might be thus attributed to<br />

polymerization shrinkage <strong>of</strong> the resin cements<br />

[20,21], combined with the coefficients <strong>of</strong> thermal<br />

expansion <strong>of</strong> the materials involved (i.e. tooth<br />

substance, cement, metal crown), during aging<br />

[22]. By contrast with the resin cements, conventional<br />

glass–ionomer cements like Fuji I are considered<br />

to be dimensionally stable during setting,<br />

and the hydrophilic <strong>for</strong>mulation <strong>of</strong> resin-modified<br />

glass–ionomer cements like Fuji Plus can compensate<br />

<strong>for</strong> the initial setting contraction by subsequent<br />

expansion due to water uptake. This<br />

difference in chemical behavior might explain the<br />

different microleakage results found <strong>for</strong> the two<br />

standard resin cements, the conventional glass–<br />

ionomer cement, and the resin-modified glass–<br />

ionomer cement.<br />

<strong>Microleakage</strong> was found to be most pronounced<br />

with the zinc-phosphate cement applied on preparation<br />

margins located in enamel. Zinc-phosphate<br />

cement on dentin showed the third-largest microleakage<br />

<strong>of</strong> all <strong>cementing</strong> <strong>agents</strong>. A similar trend was<br />

described by a number <strong>of</strong> authors [6–10] who<br />

compared several types <strong>of</strong> materials and observed<br />

the greatest degree <strong>of</strong> microleakage in <strong>full</strong> <strong>cast</strong><br />

<strong>crowns</strong> bonded with zinc-phosphate cements. Possible<br />

reasons <strong>for</strong> these unfavorable results <strong>for</strong> zincphosphate<br />

cements include their lack <strong>of</strong> micromechanical<br />

and especially—by contrast with all<br />

other cements investigated in this study—the<br />

absence <strong>of</strong> chemical retention on dental tissue<br />

[23] and their high solubility [24]. Comparisons<br />

<strong>of</strong> the clinical per<strong>for</strong>mance with regard to microleakage<br />

around <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> after 6 months in<br />

function showed that a zinc-phosphate cement<br />

(Flecks; Mizzy, Cherry Hill, NJ, USA) showed<br />

significantly higher values than a resin-modified<br />

glass–ionomer cement (Infinity; Den Mat Corp.,<br />

Santa Maria, CA, USA) [25]. It must be noted,<br />

however, that Kydd et al. [26] have shown that


<strong>Microleakage</strong> <strong>of</strong> <strong>various</strong> <strong>cementing</strong> <strong>agents</strong> <strong>for</strong> <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> 451<br />

crown restorations bonded with zinc-phosphate<br />

cement remained functional despite microleakage<br />

<strong>for</strong> over 20 years, with none <strong>of</strong> the tooth–crown<br />

interfaces revealing carious lesions. Other authors<br />

concluded that the cement dissolving at the<br />

marginal gap does not seem to have any serious<br />

consequences and does not give rise to carious<br />

penetration [27,28].<br />

In the present study, microleakage occurred<br />

exclusively at the cement–enamel/dentin interface.<br />

This observation is confirmed by <strong>various</strong><br />

studies in vitro and in vivo [9,17,25,26,29,30].<br />

Although no microleakage occurred at the metal–<br />

cement interface, the use <strong>of</strong> metal primer should<br />

be taken into consideration clinically when metal<br />

restorations are cemented using polymer-based<br />

cements, because there is a chance <strong>of</strong> a better<br />

marginal seal when using metal primer [31,32].<br />

However, this effect is mainly dependent on the<br />

combination <strong>of</strong> alloy composition, metal surface<br />

treatment [33], metal primer, and the cement used<br />

[31,32].<br />

Our analysis <strong>of</strong> microleakage in enamel versus<br />

dentin revealed statistically significant differences<br />

in all study groups, i.e. the degree <strong>of</strong> microleakage<br />

was invariably higher with preparation margins in<br />

dentin than in enamel. This result is in keeping with<br />

the observations <strong>of</strong> other authors [8,9]. Although the<br />

retention mechanism on both dentin and enamel is<br />

micromechanical in nature, both substrates are<br />

dissimilar in composition and structure. The bond<br />

between the <strong>cementing</strong> agent and the dentinal hard<br />

tissue is compromised by the tubular microstructure,<br />

the higher content <strong>of</strong> organic material, and the<br />

intrinsic humidity <strong>of</strong> the dentinal substrate [34]. It<br />

must be noted, however, that bonding properties<br />

and tracer penetration may vary from location to<br />

location, depending on the structure and composition<br />

<strong>of</strong> the enamel or dentinal substrate. Major<br />

determinants include age, location, tissue health,<br />

and dietary factors [35,36].<br />

To be able to per<strong>for</strong>m an immediate relative<br />

comparison between the in vitro results <strong>of</strong> the study<br />

groups, margins were examined only after autopolymerization<br />

<strong>for</strong> all resin cements. One would have<br />

to take into consideration, however, that lightpolymerization<br />

increases the bond between dualcure<br />

resin cements and dental restorative materials<br />

[37]. Dual-cure resin cements should there<strong>for</strong>e be<br />

polymerized with a polymerizing light, especially if<br />

the crown margins are located supragingivally and<br />

are accessible.<br />

The mean results in terms <strong>of</strong> marginal gap on<br />

storing the specimens in water <strong>for</strong> 4 weeks and<br />

subjecting them to 5000 thermocycles were least<br />

favorable <strong>for</strong> one standard dual-cure resin<br />

cement (Panavia F) and <strong>for</strong> the self-adhesive<br />

resin cement (RelyX Unicem). On the other hand,<br />

the second-most favorable marginal gaps were<br />

also obtained with resin cement (RelyX ARC).<br />

Consequently, the marginal gap quality <strong>of</strong> a given<br />

type <strong>of</strong> <strong>cementing</strong> agent may be co-determined<br />

by its specific physicochemical properties. Gemalmez<br />

et al. [38] demonstrated that the marginal<br />

gap <strong>of</strong> porcelain inlays was larger when a dualcure<br />

resin cement was used <strong>for</strong> bonding. White<br />

and Kipnis [39], who investigated the effect <strong>of</strong><br />

five different luting <strong>agents</strong> on the marginal fit <strong>of</strong><br />

<strong>cast</strong> single-crown restorations bonded to<br />

extracted premolars in vitro, observed no significant<br />

marginal gap differences in the pre-bonding<br />

stage (range 35.1–69.5 mm), but reported that<br />

significant differences did emerge after cementation.<br />

The smallest gaps were observed with a<br />

glass–ionomer cement (Ketac-Cem; 3 M ESPE,<br />

Seefeld, Germany; 82.8G12.6 mm), the largest<br />

gaps with a micr<strong>of</strong>illed resin cement (Thin Film<br />

Cement; Den Mat Corp., Santa Maria, CA, USA)<br />

using oxalate dentin bonding (333.1G45.9 mm).<br />

This finding may conceivably be due to resin<br />

cements rapidly gaining viscosity in the process<br />

<strong>of</strong> curing. For this reason, White et al. [8]<br />

recommended that resin cements should be<br />

applied swiftly and care<strong>full</strong>y in clinical practice,<br />

and that indirect restorations should be inserted<br />

with considerable pressure.<br />

The present study also showed that bonding <strong>of</strong><br />

the restorations with the zinc-phosphate cement<br />

(Harvard cement), the conventional glass–ionomer<br />

cement (GC Fuji I), the resin-modified glass–<br />

ionomer cement (GC Fuji Plus), and one <strong>of</strong> the<br />

standard resin cements (RelyX ARC), involved no<br />

significant marginal gap differences. White et al.<br />

[29] demonstrated in vivo that the marginal gaps<br />

obtained with a zinc-phosphate cement (Flecks;<br />

Mizzy, Cherry Hill, NJ, USA) and a resin-modified<br />

glass–ionomer cement (Infinity; Den Mat Corp.,<br />

Santa Maria, CA, USA) with or without dentin<br />

bonding (Tenure; Den Mat Corp.) did not significantly<br />

differ after 6 months <strong>of</strong> clinical function. The<br />

clinical implications <strong>of</strong> marginal gaps—i.e. how<br />

large they have to be to favor penetration <strong>of</strong> toxins<br />

and bacteria, pulpal damage and secondary caries—<br />

remain to be clarified.<br />

The results obtained did not show any regular<br />

influence <strong>of</strong> marginal gaps on microleakage. One<br />

would have to assume that the quality <strong>of</strong> the<br />

marginal gap obtained under the experimental<br />

conditions outlined is not correlated with the<br />

microleakage results obtained. It should be pointed<br />

out that the results <strong>of</strong> the marginal gap were<br />

smaller than the maximum clinically acceptable


452<br />

marginal gap size <strong>of</strong> 120 mm (as defined by Mc Lean<br />

and Von Frauenh<strong>of</strong>er [40]) in all test groups. As in<br />

our own study, White et al. [9] did not find any<br />

correlation between marginal gaps and microleakage.<br />

Their study examined <strong>full</strong> <strong>cast</strong> <strong>crowns</strong> made <strong>of</strong><br />

a non-precious alloy that had been cemented with a<br />

zinc-phosphate cement (Flecks; Mizzy, Cherry Hill,<br />

NJ, USA), a polycarboxylate cement (Durelon; 3M<br />

ESPE, Seefeld, Germany), a glass–ionomer cement<br />

(Ketac-Cem; 3M ESPE, Seefeld, Germany), a micr<strong>of</strong>illed<br />

resin with dentin bonding (Thin Film Cement<br />

and Tenure; Den Mat Corp., Santa Maria, CA, USA),<br />

and a resin cement (Panavia Ex; Kuraray, Osaka,<br />

Japan). Nor did the study <strong>of</strong> Lindquist and Connolly<br />

[10] find any correlation between microleakage and<br />

marginal gap when using a zinc-phosphate cement<br />

(Flecks; Mizzy, Cherry Hill, NJ, USA) and a resinmodified<br />

glass–ionomer cement (Vitremer (now<br />

RelyX Luting); 3M ESPE, Seefeld, Germany). However,<br />

more research is needed to determine the<br />

relationships between restoration-associated diseases<br />

and the variables <strong>of</strong> microleakage, marginal<br />

opening, and host factors.<br />

Although we used established protocols to<br />

simulate the oral environment, the real-life<br />

scenario is too complex to be <strong>full</strong>y reproduced<br />

by experimental set-ups <strong>of</strong> this type. On balance,<br />

it is reasonable to assume that the data obtained<br />

in the <strong>various</strong> study groups constituted a viable<br />

basis <strong>for</strong> comparison. In clinical practice, however,<br />

additional factors such as biocompatibility,<br />

thermal/electric conductivity, ease <strong>of</strong> use, and,<br />

most important, the specific requirements <strong>of</strong> each<br />

case (e.g. height <strong>of</strong> the residual tooth structure<br />

and preparation angle) must enter the equation to<br />

find out which <strong>cementing</strong> agent is most<br />

appropriate.<br />

Conclusions<br />

1. None <strong>of</strong> the <strong>cementing</strong> <strong>agents</strong> investigated in<br />

this study yielded a perfect seal at the bonding<br />

interface in enamel or dentin.<br />

2. All <strong>cementing</strong> <strong>agents</strong> investigated were associated<br />

with higher degrees <strong>of</strong> microleakage when<br />

the tooth substrate was located in dentin.<br />

3. The self-adhesive universal resin cement (RelyX<br />

Unicem) revealed the smallest degree <strong>of</strong> microleakage<br />

both in enamel and in dentin.<br />

4. After artificial aging differences in the marginal<br />

gap quality were observed.<br />

5. An association between marginal gap and microleakage<br />

was not observed.<br />

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