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discussions, stats, and author profiles for this publication at: http://www.researchgate.net/publication/275050310

Degree of conversion of dual-polymerizing

cements light polymerized through
monolithic zirconia of different thicknesses
and types
ARTICLE in THE JOURNAL OF PROSTHETIC DENTISTRY APRIL 2015
Impact Factor: 1.42 DOI: 10.1016/j.prosdent.2015.02.007 Source: PubMed

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RESEARCH AND EDUCATION

The degree of conversion of dual-polymerizing cements light

polymerized through monolithic zirconia of different
thicknesses and types
Taiseer A. Sulaiman, BDS,a Aous A. Abdulmajeed, BDS, PhD,b Terrence E. Donovan, DDS,c
Andr V. Ritter, DDS, MS, MBA,d Lippo V. Lassila, DDS, MSc,e Pekka K. Vallittu, DDS, PhD,f and
Timo O. Nrhi, DDS, PhDg
While they can be conventionally cemented to tooth preparations with adequate retention
and resistance form, airborneparticle abraded zirconia-based
restorations luted with a phosphate monomer resin-based
cement1 can offer advantages
over conventional cementation,
especially when retentive features are lost. Therefore, a
combination of mechanical and
chemical pretreatment, along
with a resin-based luting agent,
is essential for bonding to
zirconia.2
Because zirconia is a semitranslucent ceramic material
and less translucent than glass
ceramics, its thickness3,4 and
shade can affect the amount
of light transmission and
polymerizing efciency of
light-activated resin luting cements.5,6 Dual-polymerizing

ABSTRACT
Statement of problem. Monolithic zirconia restorations are increasingly common. Dual-polymerizing
cements have been advocated for cementation. The opacious nature of zirconia restoration can
attenuate light, compromising optimal resin polymerization and eventually restoration debonding.
Purpose. To evaluate the inuence of material thickness on light irradiance, radiant exposure, and
the degree of monomer conversion (DC) of 2 dual-polymerizing resin cements light-polymerized
through different brands of monolithic zirconia.
Material and methods. Dual-polymerizing resin cements (RelyX Ultimate; 3M-ESPE, and Variolink II;
Ivoclar, Vivadent) were mixed according to the manufacturers instructions with a lm thickness of 40 mm,
placed under a 1010 mm specimen of monolithic zirconia (Prettau Anterior by Zirkonzahn, Katana by
Noritake, BruxZir by Glidewell, and Zenostar by Wieland) and a zirconia core control (ICE zirkon by Zirkonzahn) at various thicknesses (0.50, 1.00, 1.50, and 2.00 mm, n=5 of each thickness). Each specimen was
irradiated for 20 seconds (RelyX Ultimate) and 40 seconds (Variolink II) with Elipar S10 (3M-ESPE, 1200 mW/
cm2). The amount of irradiance and radiant exposure was quantied for each specimen. Fourier transform
infrared spectroscopy was used to measure the DC from the bottom surface of the resin. Statistical analysis
was performed with 2-way ANOVA and post hoc Tukey honest signicant difference (HSD) tests (a=.05).
Results. Light irradiance and radiant exposure decreased as the thickness of the specimen increased
(P<.05) regardless of the brand. The ranking from least to highest was BruxZir<ICE zirkon=Wieland<Katana=Prettau Anterior. The zirconia brand, thickness, and cement type had a signicant effect
on the DC (P<.001). The DC decreased signicantly as the thickness of the zirconia increased (P<.001).
Katana and Prettau Anterior showed the highest DC and BruxZir showed the lowest.
Conclusion. The thickness of zirconia affects the DC of resin-based cements. The DC of the resin
cements differed signicantly between cements and among zirconia brands. More polymerizing
time may be needed to deliver sufcient energy through some brands of zirconia. (J Prosthet
Dent 2015;-:---)

Doctoral student, Department of Prosthetic Dentistry, University of Turku Institute of Dentistry, Turki Finland; Visiting Scholar, Department of Operative Dentistry,
University of North Carolina School of Dentistry, Chapel Hill, NC.
Assistant Professor, Department of Prosthetic Dentistry, University of Turku Institute of Dentistry, Turku, Finland.
c
Professor and Section Head of Material Science, Department of Operative Dentistry, University of North Carolina School of Dentistry, Chapel Hill, NC.
d
Professor and Chair, Department of Operative Dentistry, University of North Carolina School of Dentistry, Chapel Hill, NC.
e
Assistant Professor, Department of Biomaterials Science, University of Turku, Institute of Dentistry, Lab Manager, Turku Clinical Biomaterials Centre,
University of Turku.
f
Professor, Department of Biomaterials Science, University of Turku, Institute of Dentistry and Welfare Division, Turku, Finland.
g
Professor, Department of Prosthetic Dentistry, University of Turku, Institute of Dentistry and Clinic of Oral Diseases, Turku University Central Hospital, Turku, Finland.
b

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Issue

Table 1. Monolithic zirconia brands

Clinical Implications
Monolithic zirconia restorations attenuate light; the
amount depends on brand and thickness and affects the degree of monomer conversion. Different
resin cements have different degree of conversion.
Clinicians should be aware of the type of cement
they are using, its polymerizing time, and the energy recommended for its optimal polymerization.

luting resins combine the desirable properties of chemical

and light-polymerizing materials, providing an adequate
degree of monomer conversion (DC) beneath various
restorations. With dual polymerization, the portion of
luting resin that initially received insufcient irradiance
continues to polymerize after light exposure by means of a
delayed chemical reaction.7 If this chemical polymerization cannot compensate sufciently for the reduced
photopolymerization caused by reduced light irradiance,
insufcient hardening and a lower level of conversion of a
dual-polymerizing resin cement can lead to the early
failure of adhesively retained zirconia restorations, postoperative sensitivity, microleakage, and recurrent caries.8
It can also be associated with the release of residual
monomer, which might result in damage to surrounding
tissues.9
Limited data are available concerning the DC of resin
luting cements under monolithic zirconia restorations.
Therefore, the purpose of this study was to evaluate the
inuence of zirconia thickness on light irradiance and
radiant exposure and the DC of 2 dual-polymerizing
resin cements light-irradiated through different brands
of monolithic zirconia. The null hypothesis was that the
thickness and brand of monolithic zirconia have no effect
on light irradiance and radiant exposure, or on the DC of
dual-polymerizing resin cements.
MATERIAL AND METHODS
Monolithic zirconia specimens of 4 different brands
(Table 1) were prepared into square-shaped specimens
(1010 mm) of different thicknesses (0.50, 1.00, 1.50,
and 2.00 mm, n=5 of each thickness) with a cutting
device (Struers Secotom-50; Struers). In its green stage,
each specimen was sequentially ground to the specic
thickness with silicon carbide grinding paper (FEPA
#1200, 2400, 4000) (LaboPol 21; Struers A/S). The nal
thickness (0.01 mm) was measured with a digital
caliper (Mitutoyo Corp). The specimens were sintered
according to the manufacturers instructions by using
the manufacturers furnace for each brand. Each
specimen was polished by a single operator (T.S.) with
diamond polishers (Zircpol Plus and Zircoshine Plus;
Diatech), followed by a polishing paste (Zircon-Brite;
THE JOURNAL OF PROSTHETIC DENTISTRY

Brand Name

Manufacturer

Composition

ICE Zircon

Zirkonzahn

4-6% Y2O3, <1% Al2O3,

max. 0.02% SiO2,
max. 0.01% Fe2O3,
max. 0.04% Na2O

Prettau Anterior

Zirkonzahn

<12% Y2O3, <1% Al2O3,

max. 0.02% SiO2,
max. 0.02% Fe2O3,
max. 0.04% Na2O

BruxZir Zirconia

Glidewell
Laboratories

Unknown

Wieland Zenostar
Translucent

Ivoclar Vivadent

Unknown

Katana high
translucency
block

Kurary Noritake
Inc

(ZrO2 + HfO2 + Y2O3) >99%,

yttrium oxide (Y2O3) >4.5 e
6%,
hafnium oxide (HfO2)
5%,
other oxides
1%

Dental Ventures of America Inc) under constant pressure and for a standard time in a single directed motion, following the manufacturers instructions. The
specimens were cleaned ultrasonically in distilled water
for 15 minutes before testing (Quantrex 90; L&R Ultrasonics Manufacturing Co), and then air dried individually for 20 seconds.
Plastic rings with a 10-mm diameter opening and
thicknesses of 0.50, 1.00, 1.50, and 2.00 mm were made
to determine the light-polymerizing units irradiance
(mW/cm2) and radiant exposure (J/cm2) without a specimen. Then the light irradiance and radiant exposure
were determined through each specimen with a lightemitting diode (LED) polymerizing unit (Elipar S10; 3M
ESPE) with irradiance of 1200 mW/cm2 and wavelength
range of 430 to 480 nm (manufacturers data), and the
polymerizing time was set at 20 and 40 seconds. A calibration device (MARC Resin Calibrator; BlueLight Analytics Inc) was used to quantify the light exposure
through each specimen at the lower surface of the resin
calibrator. A custom-made jig was used to ensure the
stability and proper placement of the light-polymerizing
unit.
The dual-polymerizing resin cements used in this
study (Table 2) were mixed according to the manufacturers instructions. The translucent shade of each type of
cement was used. The DC was monitored by Fourier
transform infrared spectroscopy (Frontier; Perkin Elmer)
with a universal attenuated total reectance (ATR) sampling accessory. Two 40-mm-thick shims were placed on
each side of the ATR crystal. After mixing, the cement
was placed on the crystal and a Mylar strip was placed on
top followed by the zirconia specimen (Fig. 1). A pressure
arm was swung over the specimen and the node rotated
until it touched the specimen, and the force gauge indicated a load of 12 N, ensuring that the cement was
completely spread over the crystal without extending to
the borders of the specimen. The polymerizing time was
20 seconds for RelyX Ultimate and 40 seconds for
Sulaiman et al

2015

Table 2. Dual-polymerizing cements

Brand

Shade

RelyX Ultimate

Translucent

Variolink II

Translucent
(low viscosity)

Manufacturer

Filler vol.%

Chemical Composition

3M ESPE

43

Base: Methacrylate monomers, radiopaque silanated llers, initiator components,

stabilizers and rheological additives
Catalyst paste: Methacrylate monomers, radiopaque alkaline (basic) llers,
initiator components, stabilizers, pigments, rheological additives, uorescence dye,
dark polymerize activator for Scotchbond Universal adhesive

Ivoclar Vivadent

43.6

Base: Bis-GMA (10-25%), urethane dimethacrylate (2.5-10%), TEGDMA (2.5-10%),

inorganic ller, ytterbium triuoride, initiator, stabilizer
Catalyst: Bis-GMA (50-100%), UDMA (2.5-10%), TEGDMA (2.5-10%), inorganic ller,
ytterbium triuoride, benzoyl peroxide (<2.5%), stabilizer

Bis-GMA, bisphenol A-glycidyl dimethacrylate; UDMA, urethane dimethacrylate; TEGDMA, triethylene glycol dimethacrylate.

Table 3. Irradiance (mW/cm2) mean (SD) of groups at 10-second

polymerizing time

Light

No
Thickness Specimen
0.50 mm

0.5 mm, 1 mm,

1.5 mm, 2 mm
Shim

Zirconia specimen
Luting cement

Mylar strip

ATR sensor

Figure 1. Schematic drawing of test arrangement.

Variolink II (manufacturers instructions). The DC of each

type of cement was determined before zirconia placement as a positive control by using the same plastic rings
to control the distance between the light tip and the
cement. The cement was then polymerized through each
specimen with an LED-polymerizing unit (Elipar S10; 3M
ESPE). Immediately after polymerizing, the specimen
was shielded from ambient light and the infrared spectra
were recorded for each experimental condition (zirconia
brand, thickness, and resin cement brand). Recording
was done continuously from the bottom of the specimen
every 5.2 seconds for 15 minutes at a rate of 16 scans/
spectrum at 4 cm1 resolution using reaction kinetics
software (TimeBase V4; Perkin Elmer). Because the resin
cement presented the aliphatic bonds of the methacrylate
functional group and the aromatic vinyl bonds of
bisphenol, the DC was calculated from the aliphatic C=C
peak at 1638 cm1 and normalized against the aromatic
C=C peak at 1608 cm1 according to the formula10,11:
DC % = 1C=U 100;
where C and U are the normalized absorption peak
heights 1638 cm1 (polymerized) and 1608 cm1
Sulaiman et al

1749 (9.2)

BruxZir

Wieland ICE Zircon

564 (15.1) 664 (2.9)

726 (6.0)

Katana

Prettau
Anterior

820 (7.4) 830 (6.9)

1.00 mm 1703 (10.5) 305 (10.2) 572 (11.8) 536 (10.3) 617 (11.0) 620 (7.8)
1.50 mm

1623 (5.9)

165 (4.0)

401 (1.5)

452 (6.9)

473 (12.6) 478 (10)

2.00 mm

1292 (7.9)

103 (3.1)

360 (7.5)

352 (5.0)

381 (9.8) 400 (4.1)

(unpolymerized) materials. A new mix of cement

was placed under each specimen for a total of 5
measurements.
Statistical analysis was performed with software
(Statistical Package for the Social Sciences, v22.0; SPSS
Inc). The distribution of data was normal as determined
by the Kolmogorov-Smirnov test. Thus, the data were
analyzed with 2-way analysis of variance ANOVA (irradiance, radiant exposure, and DC as dependent variables
and zirconia brand, zirconia thickness, and cement type
as independent variables), followed by the Tukey HSD
post hoc test (a=.05). A regression analysis was performed to determine the correlation between the DC and
radiant energy for both cements.
RESULTS
The irradiance level and radiant exposure of the lightpolymerizing unit with and without zirconia specimens
are listed in Tables 3, 4. A signicant difference was
found for the amount of light irradiance and radiant
exposure through the specimens. The amount of light
irradiance and exposure decreased as the thickness of the
specimen increased (P<.05), regardless of the brand.
BruxZir showed the lowest values in terms of light
irradiance and radiant exposure and Prettau Anterior and
Katana showed the highest values. No statistically signicant difference was found between ICE zirkon and
Wieland. The ranking for the amount of light irradiance
through specimens from least to highest was: BruxZir<
ICE Zirkon=Wieland<Katana=Prettau Anterior (P<.05).
Zirconia brand, zirconia thickness, and cement type
had a signicant effect on the DC (P<.001). For any given
resin cement, Katana and Prettau Anterior showed the
highest DC, followed by Wieland, while BruxZir and ICE
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Table 4. Radiant exposure (J/cm2) (irradiance time) of groups at 20 and

40 seconds
Time

No
Specimen

BruxZir

Wieland

ICE Zircon

Katana

Prettau
Anterior

20 seconds

Issue

Table 5. DC of Rely X Ultimate under specimens at manufacturers

20-second polymerizing time, mean (SD)
Thickness ICE Zirkon

BruxZir

Wieland

Prettau
Anterior

Katana

0.50 mm

60.00 (0.68)A 60.26 (0.74)A 61.03 (0.43)AB 62.78 (0.67)B 62.78 (0.85)B

0.50 mm

35

12

13

15

17

17

1.00 mm

59.72 (0.48)A 59.73 (0.49)A 59.61 (0.41)A 61.29 (0.37)B 61.37 (0.57)B

1.00 mm

34

12

11

13

13

1.50 mm

58.06 (0.91)A 57.73 (0.77)A 58.29 (0.62)A 60.40 (0.43)B 60.87 (1.03)B

1.50 mm

32

10

10

2.00 mm

57.86 (0.85)B 55.91 (0.55)A 57.31 (0.40)AB 59.53 (0.66)C 59.90 (0.63)C

2.00 mm

26

0.50 mm

70

23

27

29

33

33

1.00 mm

68

12

23

21

25

25

1.50 mm

65

16

18

19

19

2.00 mm

52

14

14

15

16

Different superscript letters indicate different means within same row (P<.05).

40 seconds

zirkon showed the lowest DC. The DC was 63.1% for

RelyX Ultimate and 66% for Variolink II with no specimen attenuating the light. The DC of both cements are
listed in Tables 5, 6. The DC decreased signicantly as the
thickness of the zirconia increased (P<.001), regardless of
the brand. A linear regression analysis indicated a positive correlation between DC and radiant exposure (R2=
.816, RelyX Ultimate) and (R2= .710, Variolink II) P<.001
(Fig. 2).
DISCUSSION
In this study, the DC decreased signicantly as the
thickness of the zirconia increased, which should raise
the awareness of crown thickness and whether additional
exposure time is needed to deliver sufcient energy to
maximize polymerization without overheating. The DC
was signicantly different among zirconia brands with
Katana and Prettau Anterior showing higher DC than
Wieland, ICE Zircon, and BruxZir. This was in direct
correlation with the amount of irradiance and radiant
exposure. Therefore, the null hypothesis was rejected.
The irradiance, radiant exposure, and DC were affected
by the brand and thickness of the zirconia specimen.
Many factors can affect the DC of resin-based materials, including light-polymerizing time and irradiance,
indirect restoration thickness, shade, translucency, and
the temperature and viscosity of the material.12-14 The
monomer formulation, the concentrations of sensitizer,
initiator, and inhibitor have also been shown to affect the
DC.8 Composite resins based on bisphenol A diglycidyl
methacrylate (Bis-GMA) or similar monomers produce
50% to 75% DC after polymerization.15,16 However, this
does not imply that remaining monomer molecules are
left in the resin, because 1 of the 2 methacrylate groups
per dimethacrylate molecule could still be covalently
bonded to the polymer structure, forming a pendant
group. Although, a minimum clinically accepted DC has
not yet been established, all the factors mentioned can
play a role.
THE JOURNAL OF PROSTHETIC DENTISTRY

Table 6. DC of Variolink II under zirconia brands at manufacturers

40-second polymerizing time, mean (SD)
Thickness ICE Zirkon

BruxZir

Wieland

Prettau
Anterior

Katana

0.50 mm

64.11 (0.17)A 64.05 (0.30)A 65.51 (0.53)B 65.58 (0.56)B 65.51 (0.31)B

1.00 mm

62.96 (0.66)AB 62.38 (0.76)A 63.36 (0.41)AB 64.03 (0.92)BC 64.81 (0.68)C

1.50 mm

61.97 (0.52)AB 61.25 (0.52)A 63.06 (0.83)BC 64.19 (0.91)C 64.20 (0.85)C

2.00 mm

60.27 (0.40)A 60.45 (0.41)A 62.36 (1.09)B 62.54 (0.83)B 63.04 (0.74)B

Different superscript letters indicate different means within same row (P<.05).

The opacious nature of monolithic zirconia restorations can limit the amount of light transmitted through
the material. The brand and thickness of zirconia can
signicantly inuence light irradiance and radiant exposure.3,4 The amount of radiant exposure required for
optimal polymerization is presented by some manufacturers (J/cm2). In the case of Variolink II, the minimum
amount of energy for optimal polymerization of the
cement over a 40-second polymerizing period is 26 J/cm2
(Singhal S, Ivoclar Vivadent, personal communication).
Regarding RelyX Ultimate, the manufacturer did not
indicate the minimum amount of energy required for
optimal polymerization. The manufacturers instruction
of 20 seconds was followed. An attempt to determine
whether increasing the polymerizing time to 40 seconds
would affect the DC was done with no signicant increase. With the use of the MARC system, radiant
exposure and irradiance was quantied. Whether sufcient radiant exposure is being delivered can be determined by comparing the determined results with the
radiant exposure required by the manufacturer for
optimal polymerization.
It is important to know the light polymerizing units
output, beam homogeneity, irradiance, and spectral
emission. In general, polymerizing lights with high irradiance appear preferable for increasing the amount of
light reaching the dual-polymerizing resin cements.17 It
is also important to comply with optimum time of light
polymerizing. Research has shown that adequate duration of light exposure yielded higher conversion values.13
However, increasing exposure time to compensate for
any energy loss can deliver excessive energy and generate
heat, which can damage gingival tissue.18
Despite light attenuation through the zirconia
specimens, it seems that an acceptable but not optimal
Sulaiman et al

2015

66

65

65

DC (%)

DC (%)

64

63

62

63
62

61

60

64

61

10

20

Radiant Energy (J/cm2)

30

40

60

10

20

Radiant Energy (J/cm2)

30

40

Figure 2. Regression analysis. A, Positive correlation between DC and radiant exposure (R = .816, RelyX ultimate). B, Positive correlation between DC
and radiant exposure (R2= .710, Variolink II).

DC (>50%) was realized through the different brands

at the various thicknesses. The wavelength of the light
used in this study was between 420 and 480 nm.
These wavelengths can be transmitted to some degree
through the zirconia specimens. The peak absorbance
for camphorquinone (CQ) (photo initiator) is at
470 nm,18,19 allowing a resin to photopolymerize more
properly than those containing photoinitiators with
absorbance peaks of lower wavelengths.20 Both cements tested have CQ in their system, which can
explain the compatibility leading to the sufcient DC.
In situations where light is attenuated, additional
chemical polymerization of dual-polymerizing resin
cements should sufce to compensate for the limited
photopolymerization and ensure an ultimate maximum
polymerization. In the present study, the role of the
chemical polymerization might not have assisted the
cement to reach its maximum polymerization, but
rather helped in reaching a DC within an acceptable
limit. Additionally, the chemical component of 1 brand
can be more efcient in polymerizing than anothers
and that might account for why Variolink II had a
better DC than RelyX Ultimate; however, this statistically signicant difference might be clinically irrelevant. Rueggeberg and Caughman12 determined the
polymerization potential of dual-polymerizing cements
and found that it varies greatly according to the brand
used.
The use of at zirconia specimens was a limitation of
this study but enabled placement of the light tip on the
surface, in contrast to the clinical situation where occlusal
cusps can place the tip further from the cement. This
decreases the irradiance and radiant exposure further.
Increasing the distance of the light tip away from the
Sulaiman et al

resin-based material can have a negative effect on the

degree of monomer conversion.21-23 Therefore, the DC of
the resin cements under anatomic crowns might have
lower values than in the corresponding in vitro
experiment.
To further comprehend the polymerization process in
dual-polymerizing cements, the ratio and chemistry between the light polymerizing and the chemical polymerizing components must be understood. However, the
attainment of a signicant chemically induced continuation of polymerization after light polymerizing is difcult
to achieve.12 The initial light exposure causes a rapid
increase in the conversion of the resin, resulting in a
viscous gel. This rapid increase in viscosity hinders the
migration of active radical components that would be
responsible for the further chemically induced polymerization.24 In light-polymerizing or dual-polymerizing
resin composites, 90% of the DC measured after 24 hours
develops within the rst 10 minutes.12 Therefore, in the
present study, an experimental period of 15 minutes
(with 3-minute interval readings representing the DC of
both polymerization mechanisms), corresponding to the
initial setting phase, is likely sufcient and clinically
relevant for estimating the setting characteristics of the
dual-polymerizing cements.
It would have been of further interest to determine
the hardness of the resin cement (such as with a Knoop
Hardness Test) to determine any correlation between the
DC and hardness of the cement. Also, the DC was
determined at room temperature (23 C). Under clinical
situations, the higher intraoral temperature (37 C) can
increase the rate of the DC.14 Further research and
controlled clinical trials should be conducted before any
clinical recommendations can be given.
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CONCLUSIONS
Based on the ndings of this study, the following can be
concluded:
1. Monolithic zirconia restorations attenuate light; the
amount depends on the brand and thickness, and
can affect the radiant exposure delivered to the
resin-based cement, compromising polymerization.
2. The DC of resin cements can decrease signicantly
under monolithic zirconia restorations but seems to
be within the accepted range of more than 50%.
3. Different resin cements can have a different DC.
The type of cement, polymerizing time, and energy
affect polymerization.
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Corresponding author:
Dr Taiseer A. Sulaiman
University of North Carolina
5405F Koury Oral Health Science Bldg, CB 7450
Chapel Hill, NC 27599
Email: sulaiman@unc.edu
Acknowledgments
The author thanks Dr Anna Paula Beltrame for statistical support and Dr Awab A.
Abdulmajeed for laboratory support.
Copyright 2015 by the Editorial Council for The Journal of Prosthetic Dentistry.

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