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Received 5 November 2003; received in revised form 1 June 2004; accepted 13 July 2004
KEYWORDS Summary Objectives. To evaluate microleakage and marginal gaps in full cast
Cementing agent; crown restorations bonded with six different types of cementing agents.
Microleakage; Methods. Sixty non-carious human premolars and molars were prepared in a
Marginal gap; standardized manner for full cast crown restorations. The mesial and distal margins
Full cast crowns were located in dentin, while the vestibular and palatal/lingual margins were located
in enamel. Crowns were made from a high-gold alloy using a standardized technique.
The specimens were randomized to six groups of cementing agents: one zinc-
phosphate cement (Harvard cement), one conventional glass–ionomer cement (Fuji
I), one resin-modified glass–ionomer cement (Fuji Plus), two standard resin cements
(RelyX ARC, Panavia F), and one self-adhesive universal resin cement (RelyX
Unicem). After 4 weeks of storage in distilled water at 37 8C, the specimens were
subjected to 5000 thermocycles ranging from 5 to 55 8C. Then, they were placed in a
silver nitrate solution, embedded in resin blocks, and vertically cut in buccolingual
and mesiodistal direction. Subsequently, the objects were evaluated for micro-
leakage and marginal gap using a high-resolution digital microscope camera.
Results. A number of inter-group differences were statistically significant. RelyX
Unicem showed the smallest degree of microleakage both in enamel and in dentin.
Panavia F und RelyX Unicem were associated with significantly larger marginal gaps
than all other cementing agents. No association was observed between microleakage
and marginal gap other than a weak direct correlation when using Harvard cement on
enamel.
Significance. The cementing agents investigated revealed different sealing
abilities. These differences were not associated with specific types of materials.
Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Introduction
related to pulpal problems [2,3], hypersensitivity, distilled water at room temperature immediately
and secondary caries [4], the latter being the most after extraction. Calculus and residual periodontal
common reason why restorations are replaced [5]. tissue were removed using a surgical knife, scaler,
Few studies have dealt with microleakage in full and curette. Subsequently, the teeth were con-
cast crowns based on different types of cementing servatively polished using a rotating brush and
agents [6–10]. Moreover, the methodologies and pumice.
cementing agents used in these studies have been The preparations for the full cast crowns were
too diverse to allow direct comparison of the data. performed using a suitable design and a converging
But it is possible to analyze different types of angle of around 68 to achieve optimal retention and
commercially available cementing agents that can resistance properties. The occlusal and axial sur-
be used for long-term cementation of fixed restor- faces were reduced by approximately 1.2 and
ations. These include zinc-phosphate cements, 0.8 mm, respectively. The cervical preparation
conventional glass–ionomer cements, resin-modi- margins were designed as circular chamfers using
fied glass–ionomer cements, standard resin torpedo-shaped diamond burs and water-cooling
cements, and a recently developed material (Gebr. Brasseler, Lemgo, Germany; No. 878,314,
described as self-adhesive universal resin cement. size 012). The preparations were finished with the
The objective in developing this cement was to help of magnifying loupes (magnification !3.5;
combine the ease of handling offered by glass– Zeiss, Oberkochen, Deutschland; serial #53-20)
ionomer cements with the favorable mechanical using fine and extra-fine diamond burs (Gebr.
properties [11], attractive esthetics [12], and good Brasseler, Lemgo, Germany; No. 8878.314 and
adhesion of resin cements [13]. 878EF.314, size 012). Subsequently, a final check
A review of the literature by Raskin et al. [14] of the preparations was performed. The mesial and
showed that 62.5% out of 144 studies on micro- distal margins were located in dentin, while the
leakage performed between 1992 and 1998 eval- vestibular and palatal/lingual margins were located
uated microleakage in Class V cavities, while only in enamel.
4.3% evaluated microleakage and marginal gaps as For the model dies, impressions of the prepared
study parameters involved in crown restorations. teeth were taken with Impregum Penta (3M ESPE,
These latter include only a limited number of Seefeld, Germany) and poured with Type IV resin-
studies [9,10] investigating the correlation between stabilized extra-hard stone (esthetic-base 300;
microleakage and marginal gaps in full cast crowns; dentona AG, Dortmund, Germany; lot #51001742)
no such correlation was found. However, the following the manufacturer’s mixing instructions.
significance of the marginal gaps of full cast The stone was allowed to set for 40 min and then
restorations and their clinical consequences remain removed from the impression. The resultant stone
to be determined. dies were trimmed and covered with stone hard-
The objective of the present in vitro study was to ener (Classic Hardener Spacer clear; Kerr Lab, Belle
investigate microleakage and marginal gaps associ- de St Claire, France) followed by two layers of die
ated with cementing agents in full cast crowns spacer (Classic Cement Spacer blue; Kerr Lab, Belle
following artificial aging. Other questions to be de St Claire, France) above the preparation margin.
examined were (1) whether various types of The preparation margin was marked with a non-
cementing agents produce the same sealing ability graphite pencil under a stereomicroscope at !32
for definite bonding of indirect restorations and (2) magnification (Zeiss, Oberkochen, Germany; Stemi
in how far microleakage results differ depending on 2000-C, serial #2004003753). Subsequently, red
whether the margins of the restoration are placed in cervical wax and blue modeling wax (YETI Dental-
dentin or in enamel. A final objective was to produkte, Engen, Germany) were used to model full
determine whether there was a connection between crowns of 0.5 mm thickness. Four round reference
microleakage and marginal gaps in full cast crowns. marks approximately 1.5 mm in diameter were
applied in the mesial, distal, vestibular and
lingual/palatal segments centrally around 3 mm
above the preparations located in enamel and
Materials and Methods dentin. Five wax copings each were embedded in
a #3 muffle ring with phosphate-bonded investment
Specimen preparation (Precibalite plus; Dentona AG, Dortmund,
Germany; lot #0501101). After setting, the muffle
A total of 60 freshly extracted non-carious perma- was heated and a centifugal casting performed
nent human molars with fully developed roots were using a Type IV high-gold casting alloy (Portadur P4;
selected for this study. All teeth were stored in Wieland Edelmetalle GmbH, Pforzheim, Germany;
Microleakage of various cementing agents for full cast crowns 447
relative constituents: Au 68.5%, Ag 12.0%, Cu 12.0%, (GC Fuji Plus and RelyX Unicem) were supplied
Pt 6.9%, Zn 0.5%, Ir 0.1%; lots #4492 and 4269). in pre-measured capsules. Upon activation, these
The castings were divested, trimmed and seated materials were mechanically triturated with the
using well-established procedures routinely used by rotational mixing machine (CapMix; 3M ESPE,
dental laboratories for crown restorations. The fit Seefeld, Germany) for the time recommended by
of the castings was checked with silicone (Fit the manufacturers (10 or 15 s). RelyX ARC was
Checker; GC, Munich, Germany) and improved if supplied in pre-measured delivery systems. Pana-
necessary. Any points visibly pressed into the via F was mixed on a mixing block, using a hard
silicone were relieved using a small (0.08 mm in plastic spatula, at a base-to-catalyst paste ratio of
diameter) rotary instrument. The marginal fit of all 1:1 for approximately 20 s. An oxygen-blocking gel
castings was verified on the prepared residual teeth (Oxyguard II; Kuraray, Osaka, Japan; lot #00373A)
under a stereomicroscope (!32 magnification) and was applied for 3 min when Panavia F was used.
with an extra-fine probe (EXD5; Hu-Friedy, Chicago, Fuji I was manually mixed at a powder-to-liquid
IL, USA). Subsequently, the interior surface of the ratio of 1.8–1.0 for around 20 s. The powder-to-
gold frameworks was sandblasted with Al2 O 3 liquid ratio of Harvard cement was determined by
(Hasenfratz, Grafing, Germany; average grain weighing according to the manufacturer’s instruc-
size, 105 mm; pressure, 0.18 MPa; distance, tions using an analytical balance (G1 mg). Mixing
10 mm; duration, 10 s). was performed on a cool slab, over a wide area,
Our experimental set-up included one zinc- to incorporate small increments of powder into
phosphate cement (Harvard cement), one conven- the liquid for approximately 90 s (Harvard
tional glass–ionomer cement (Fuji I), one resin- cement).
modified glass–ionomer cement (Fuji Plus), two Before cementation, all 60 teeth were random-
standard dual-cure resin cements (RelyX ARC, ized along with their gold frameworks to six test
Panavia F), and one recently developed dual- groups (nZ10). The interior surfaces of the crown
cure self-adhesive resin cement (RelyX Unicem) restorations and the prepared teeth were cleaned
(Table 1). All cementing agents were processed with alcohol. All teeth, which were to receive the
at room temperature (23 8C) strictly following resin-modified glass–ionomer cement or a standard
the manufacturers’ instructions. Two cements resin cement, were pretreated with dentin
adhesives as recommended by the manufacturers potential calibration-related error due to the width
(Table 1). Dentin adhesives were not used for the of mapped lines was G0.709 or G0.475% depending
zinc-phosphate cement, the conventional glass– on the magnification factor relative to the absolute
ionomer cement, and the self-adhesive resin measured values. Depending on the magnification,
cement. Bonding was performed by loading the 2.42 or 3.64 mm/pixel were obtained. Metric assess-
cementing agent into the interior surface of the ment of distances was performed using micrometers
restoration and applying finger pressure for 10 s. (mm) as units. A randomly selected image including
Then the frameworks were axially loaded at a 10 measurements was analyzed to determine the
constant weight of 58.8 N for 7 min [15]. Excess potential mapping error due to the definition of
cement was removed with a scaler; marginal fit was microleakage length. Given a measured length of
checked both by visual inspection and with a probe. 1 mm, a maximum mapping error of G0.01 mm was
All tooth-restoration specimens were stored in obtained irrespective of the magnification factor.
distilled water at 37 8C for 4 weeks, then they were Marginal gaps were measured as defined by
subjected to 5000 thermocycles ranging from 5 to Holmes et al. [18] using the stereomicroscope
55 8C (immersion time, 20 s; transfer time, 10 s). (4730129901; Zeiss, Oberkochen, Germany) and
Subsequently, the root surfaces of the restored digital microscope camera. The selected magnifi-
teeth were covered with two layers of nail varnish cation was based on 1.21 mm equaling one pixel.
(ending 2 mm below the crown margin) and sub- Based on the absolute values measured, the
jected to silver nitrate penetration [16]. Then maximum calibration-related error was G0.154%.
they were placed into an unimolar silver nitrate A randomly selected image including 10 measure-
solution (Crystal, Fisher Scientific, Fairfield, NJ, ments was analyzed to determine the potential
USA) for 6 h, followed by thorough rinsing, storage mapping error due to the definition of marginal gap
in a photochemical developer (Solutek Corporation, length. Given a length of 40 mm, a maximum
Boston, MA, USA) for 12 h, and exposure to a 150-W mapping error of G0.18 mm was obtained.
floodlamp for 6 h.
Next, the tooth-restoration specimens were Statistical analysis
embedded in a transparent resin matrix (Buehler
Epoxide; Buehler, Lake Bluff, IL, USA), which was Descriptive representation of continuous variables
allowed to harden at room temperature for 24 h. was based on mean values, SD, and minimum–
Each resin block was cut twice in the buccolingual maximum values. In addition, a number of tests
and the mesiodistal direction along the previously (skewness test, kurtosis test, and omnibus test)
applied reference marks using a slow-speed diamond were used to analyze whether the frequency
saw (Isomet; Buehler Ltd, Evanston, IL, USA) with distribution of the random sample differed signifi-
water-cooling. In this way, each specimen featured cantly from the normal distribution. Since, the bulk
eight surfaces (four in enamel and four in dentin) for of data was not characterized by a normal
analysis of microleakage and marginal gap. The cut distribution, a non-parametric Kruskal–Wallis test
surfaces were once again placed under a 150-W was used to analyze differences in the various
floodlamp for 5 min, such that all portions of the groups of cementing agents, comparing the
silver nitrate penetration acquired a black color. obtained test parameters (Bonferroni-corrected p
values). A non-parametric Wilcoxon’s test was used
to evaluate the differences between enamel and
Evaluation of microleakage and marginal gap
dentinal substrates. The selected level of statistical
using a high-resolution digital microscope significance was p!0.05. Spearman’s correlation
camera coefficient (R) was used to assess the correlation
between two continuous variables.
The microleakage in the area of the tooth–cement
interface was defined as linear penetration of silver
nitrate starting from the restorative crown margins
[17] and was determined with a stereomicroscope Results
(475052-9901; Zeiss, Oberkochen, Germany) and
AxioCam HR digital microscope camera (Zeiss, Microleakage with preparation margins
Oberkochen, Germany; software module: Axio in enamel
Vision 3.1). The images were taken at a resolution
of 1300!1030 pixels. A micrometer scale (474026; Fig. 1 illustrates the mean values and SD for the
Zeiss, Oberkochen, Germany) was placed diagonally microleakage findings obtained with the various
across the image for calibration. The maximum cementing agents. The smallest degree of
Microleakage of various cementing agents for full cast crowns 449
Figure 1 Mean values and SD for microleakage, based Figure 2 Mean values and SD for microleakage, based
on 40 measurements for each material, with preparation on 40 measurements for each material, with preparation
margins located in enamel. margins located in dentin.
microleakage was observed with the dual-cure self- the standard resin cement RelyX ARC and the self-
adhesive resin cement (RelyX Unicem; 0.70G adhesive resin cement RelyX Unicem (p!0.0001),
0.61 mm), followed by the conventional glass– and between the standard resin cement Panavia F
ionomer cement (Fuji I; 0.71G0.32 mm), and the and the self-adhesive resin cement RelyX Unicem
resin-modified glass–ionomer cement (Fuji Plus; (p!0.0001).
0.77G0.48 mm). The greatest degree of microleak-
age was observed with the zinc-phosphate (Har- Microleakage with preparation margins in
vard) cement (1.59G0.64 mm). The Kruskal–Wallis
enamel versus dentin
test revealed statistically significant differences
between the zinc-phosphate (Harvard) cement on
All test groups revealed significant differences in
one hand and all other agents (all p!0.01) with the
microleakage between enamel and dentin. Micro-
exception of standard resin cement (RelyX ARC) on
leakage was invariably more pronounced in dentin
the other. A significant difference was also estab-
than in enamel (Table 2).
lished between one standard resin cement (RelyX
ARC) and the self-adhesive resin cement (RelyX
Unicem) (pZ0.019). Marginal gap
crown restorations bonded with zinc-phosphate cement (Panavia F) and for the self-adhesive
cement remained functional despite microleakage resin cement (RelyX Unicem). On the other hand,
for over 20 years, with none of the tooth–crown the second-most favorable marginal gaps were
interfaces revealing carious lesions. Other authors also obtained with resin cement (RelyX ARC).
concluded that the cement dissolving at the Consequently, the marginal gap quality of a given
marginal gap does not seem to have any serious type of cementing agent may be co-determined
consequences and does not give rise to carious by its specific physicochemical properties. Gemal-
penetration [27,28]. mez et al. [38] demonstrated that the marginal
In the present study, microleakage occurred gap of porcelain inlays was larger when a dual-
exclusively at the cement–enamel/dentin inter- cure resin cement was used for bonding. White
face. This observation is confirmed by various and Kipnis [39], who investigated the effect of
studies in vitro and in vivo [9,17,25,26,29,30]. five different luting agents on the marginal fit of
Although no microleakage occurred at the metal– cast single-crown restorations bonded to
cement interface, the use of metal primer should extracted premolars in vitro, observed no signifi-
be taken into consideration clinically when metal cant marginal gap differences in the pre-bonding
restorations are cemented using polymer-based stage (range 35.1–69.5 mm), but reported that
cements, because there is a chance of a better significant differences did emerge after cementa-
marginal seal when using metal primer [31,32]. tion. The smallest gaps were observed with a
However, this effect is mainly dependent on the glass–ionomer cement (Ketac-Cem; 3 M ESPE,
combination of alloy composition, metal surface Seefeld, Germany; 82.8G12.6 mm), the largest
treatment [33], metal primer, and the cement used gaps with a microfilled resin cement (Thin Film
[31,32]. Cement; Den Mat Corp., Santa Maria, CA, USA)
Our analysis of microleakage in enamel versus using oxalate dentin bonding (333.1G45.9 mm).
dentin revealed statistically significant differences This finding may conceivably be due to resin
in all study groups, i.e. the degree of microleakage cements rapidly gaining viscosity in the process
was invariably higher with preparation margins in of curing. For this reason, White et al. [8]
dentin than in enamel. This result is in keeping with recommended that resin cements should be
the observations of other authors [8,9]. Although the applied swiftly and carefully in clinical practice,
retention mechanism on both dentin and enamel is and that indirect restorations should be inserted
micromechanical in nature, both substrates are with considerable pressure.
dissimilar in composition and structure. The bond The present study also showed that bonding of
between the cementing agent and the dentinal hard the restorations with the zinc-phosphate cement
tissue is compromised by the tubular microstruc- (Harvard cement), the conventional glass–ionomer
ture, the higher content of organic material, and the cement (GC Fuji I), the resin-modified glass–
intrinsic humidity of the dentinal substrate [34]. It ionomer cement (GC Fuji Plus), and one of the
must be noted, however, that bonding properties standard resin cements (RelyX ARC), involved no
and tracer penetration may vary from location to significant marginal gap differences. White et al.
location, depending on the structure and compo- [29] demonstrated in vivo that the marginal gaps
sition of the enamel or dentinal substrate. Major obtained with a zinc-phosphate cement (Flecks;
determinants include age, location, tissue health, Mizzy, Cherry Hill, NJ, USA) and a resin-modified
and dietary factors [35,36]. glass–ionomer cement (Infinity; Den Mat Corp.,
To be able to perform an immediate relative Santa Maria, CA, USA) with or without dentin
comparison between the in vitro results of the study bonding (Tenure; Den Mat Corp.) did not signifi-
groups, margins were examined only after autopo- cantly differ after 6 months of clinical function. The
lymerization for all resin cements. One would have clinical implications of marginal gaps—i.e. how
to take into consideration, however, that light- large they have to be to favor penetration of toxins
polymerization increases the bond between dual- and bacteria, pulpal damage and secondary caries—
cure resin cements and dental restorative materials remain to be clarified.
[37]. Dual-cure resin cements should therefore be The results obtained did not show any regular
polymerized with a polymerizing light, especially if influence of marginal gaps on microleakage. One
the crown margins are located supragingivally and would have to assume that the quality of the
are accessible. marginal gap obtained under the experimental
The mean results in terms of marginal gap on conditions outlined is not correlated with the
storing the specimens in water for 4 weeks and microleakage results obtained. It should be pointed
subjecting them to 5000 thermocycles were least out that the results of the marginal gap were
favorable for one standard dual-cure resin smaller than the maximum clinically acceptable
452 A. Piwowarczyk et al.
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