d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

Available online at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Depth of cure of resin composites: Is the ISO 4049 method

suitable for bulk ll materials?
Simon Flury a, , Stefanie Hayoz b , Anne Peutzfeldt a , Jrg Hsler b , Adrian Lussi a
a
b

Department of Preventive, Restorative and Pediatric Dentistry, School of Dental Medicine, University of Bern, Switzerland
Institute of Mathematical Statistics and Actuarial Science, University of Bern, Switzerland

a r t i c l e

i n f o

a b s t r a c t

Article history:

Objectives. To evaluate if depth of cure DISO determined by the ISO 4049 method is accurately

Received 6 October 2011

reected with bulk ll materials when compared to depth of cure Dnew determined by Vickers

Received in revised form

microhardness proles.

7 February 2012

Methods. DISO was determined according to ISO 4049; Depth of cure and resin composite

Accepted 7 February 2012

specimens (n = 6 per group) were prepared of two control materials (Filtek Supreme Plus,
Filtek Silorane) and four bulk ll materials (Surel SDR, Venus Bulk Fill, Quixl, Tetric EvoCeram Bulk Fill) and light-cured for either 10 s or 20 s. For Dnew , a mold was lled with one

Keywords:

of the six resin composites and light-cured for either 10 s or 20 s (n = 22 per group). The mold

Increment

was placed under a microhardness indentation device and hardness measurements (Vickers

Light-curing time

hardness, VHN) were made at dened distances, beginning at the resin composite that had

Restorative

been closest to the light-curing unit (i.e. at the top) and proceeding toward the uncured
resin composite (i.e. toward the bottom). On the basis of the VHN measurements, Vickers
hardness proles were generated for each group.
Results. DISO varied between 1.76 and 6.49 mm with the bulk ll materials showing the highest
DISO . Dnew varied between 0.2 and 4.0 mm. Dnew was smaller than DISO for all resin composites
except Filtek Silorane.
Conclusions. For bulk ll materials the ISO 4049 method overestimated depth of cure compared to depth of cure determined by Vickers hardness proles.
2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1.

Introduction

Energy of the light emitted from a light-curing unit decreases

drastically when transmitted through resin composite [1],
leading to a gradual decrease in degree of conversion of the
resin composite material at increasing distance from the irradiated surface. Decreases in degree of conversion compromise
physical properties and increase elution of monomer [25] and
thus may lead to premature failure of a restoration or may
negatively affect the pulp tissue. When restoring cavities with

light-curing resin composites, it has therefore been regarded

as the gold standard to apply and cure the resin composite
in increments of limited thickness. The maximal increment
thickness has been generally dened as 2 mm [6,7]. However,
restoring cavities, especially deep ones, with resin composite
increments of 2 mm thickness is time-consuming and implies
a risk of incorporating air bubbles or contaminations between
the increments. Thus, various manufacturers have recently
introduced new types of resin composites, so-called bulk ll
materials, which are claimed to be curable to a maximal increment thickness of 4 mm [811].

Corresponding author at: Freiburgstrasse 7, CH-3010 Bern, Switzerland. Tel.: +41 316322581; fax: +41 316329875.
E-mail address: simon.ury@zmk.unibe.ch (S. Flury).
0109-5641/$ see front matter 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2012.02.002

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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

A method for dening the maximal increment thickness

of resin composites has been introduced by the International
Organization for Standardization ISO in the second edition
of ISO 4049 in the year 1988 [12]. The method is ofcially
denominated as ISO 4049; Depth of cure, and according to
the method the resin composite to be tested is lled in a
tube-shaped mold, light-cured, pushed out of the mold, and
uncured resin composite material is then removed (scraped
away) with a spatula leaving a hard cylindrical specimen.
Finally, the absolute length of this hard specimen is measured and divided by two. The resulting value is recorded as
the depth of cure and denes the maximum increment thickness. The rationale for the division factor two is that not all
the hardened specimen is actually optimally cured [2,13,14].
The ISO 4049 method was developed using a microlled resin
composite (Durall, Kulzer & Co GmbH, Bad Homburg, West
Germany) [15], one of the rst visible light-curing resin composites. Ever since, the principle of the ISO 4049 method has
basically remained the same [16].
Resin composites, however, have undergone continuous
development through the years as regards their various components, e.g. the ller and the initiator. It seems likely that
the new bulk ll materials have required certain changes or
modications in the composition, and it is therefore relevant
to verify the accuracy of the ISO 4049 method and its division
factor.
Since hardness measurement has been shown to be a practical method to indirectly determine degree of conversion for
a given resin composite [14,1720], hardness proles can be
used to alternatively measure depth of cure. Consequently,
the aim of this study was to evaluate if depth of cure determined by the ISO 4049 method is accurately reected with bulk
ll materials when compared to depth of cure determined by
Vickers hardness proles. In order to arrive at this aim several subaims were set: (1) to determine the depth of cure by
ISO 4049, (2) to measure Vickers hardness at increasing distances from the light-curing source, (3) to determine at which
depth 80% of the maximum Vickers hardness was obtained,
and (4) to determine which division factor should be used to
arrive at this 80% of maximum Vickers hardness depth. The
overall hypothesis to be tested was that the ISO 4049 method
accurately reects the depth of cure determined by Vickers
hardness estimations of the degree of conversion.

2.

Materials and methods

Six resin composites (Table 1) were used for investigating the

accuracy of the ISO 4049 method: Two control materials (Filtek Supreme Plus and Filtek Silorane), two owable bulk ll
materials (Surel SDR and Venus Bulk Fill), and two highviscosity bulk ll materials (Quixl and Tetric EvoCeram Bulk
Fill). All light-curing was performed with an LED light-curing
unit (Demi, Kerr Corporation, Middleton, WI, USA) and light
power density was veried to be at least 1000 mW/cm2 at the
beginning and end of each day of specimen preparation with
a radiometer (Demetron L.E.D. Radiometer, Kerr Corporation).

2.1.

Depth of cure by ISO 4049

Depth of cure by ISO 4049 was performed with re-usable stainless steel molds according to ISO 4049:2000 [16]. Pretests had
found the absolute length of cylindrical specimens of the
cured resin composite to vary between 3.5 and 13 mm depending on the resin composite. The ISO 4049 method states that
the stainless steel molds shall be at least 2 mm longer than the
absolute length of the cylindrical specimens. Thus, stainless
steel molds of 6 mm, 9 mm, or 15 mm in length and an internal
diameter of 4 mm were custom-made.
Depending on the resin composite, the mold of either
6 mm, 9 mm, or 15 mm in length was placed on a glass slide
covered by a Mylar strip (Hawe Stopstrip Straight, KerrHawe,
Bioggio, Switzerland). The mold was then lled in bulk with
one of the six resin composites. The top side of the mold was
covered with a second Mylar strip and the resin material made
ush with the mold by use of a second glass slide. The mold
was placed on white lter paper (Filter Paper Circles 589/1,
Schleicher & Schuell MicroScience GmbH, Dassel, Germany).
The second glass slide was removed and the resin composite was light-cured for either 10 s or 20 s keeping the light tip
centered and in contact with the second Mylar strip. After
light-curing, the cylindrical specimens were pushed out of the
mold and the uncured resin composite material was removed
with a plastic spatula. The absolute length of the cylindrical
specimens of cured resin composite was then measured with a
digital caliper of 0.01 mm accuracy (Mitutoyo IP 65, Kawasaki,
Japan). The absolute length (AL) was divided by two and the
latter value recorded as DISO . Six specimens were made in each
of the 12 groups (i.e. six materials light-cured for either 10 s or
20 s).

2.2.

Depth of cure by Vickers hardness proles

Depth of cure by Vickers hardness proles was performed in

a re-usable, block-shaped, and custom-made stainless steel
mold with a semicircular notch of 15 mm in length and 4 mm
in diameter (Fig. 1A). The semicircular notch was entirely lled
with one of the six resin composites. Then, the mold was covered with a Mylar strip (Hawe Stopstrip Straight, KerrHawe)
and the resin composite was made ush with the mold by
use of a glass slide. Excess resin material was removed and
the mold was covered by a stainless steel shell (Fig. 1B). A
second Mylar strip was placed on the semicircular opening
(Fig. 1C) and the resin composite was light-cured through
the semicircular opening (top surface) for 10 s or 20 s keeping
the light tip centered and in contact with the second Mylar
strip. After light-curing, the shell and both Mylar strips were
removed (Fig. 1D) and the mold including the resin composite specimen was placed under a microhardness indentation
device (Fischerscope HM2000, Helmut Fischer GmbH, Sindelngen, Germany). Subsequently, hardness measurements
(Vickers hardness, VHN) were made on the resin composite specimen at dened distances, beginning with the resin
composite which had been closest to the light tip (i.e. from
the top) and moving toward the uncured resin composite
(i.e. toward the bottom) until VHN of the resin composite could not be measured anymore due to its softness. The
dened distances () were: 0.1 mm, 0.2 mm, 0.5 mm, 1.0 mm,

523

d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

Table 1 Resin composites used.

Resin composite

Type of resin composite

(according to
manufacturer)

Maximum increment
thickness (mm) (according
to manufacturer)

Shade

LOT-number

Filtek Supreme Plus

3 M ESPE, St. Paul,
MN, USA
Filtek Silorane
3 M ESPE, St. Paul,
MN, USA
Surel SDR
Dentsply Caulk,
Milford, DE, USA
Venus Bulk Fill
Heraeus Kulzer,
Hanau, Germany
Quixl
Dentsply DeTrey,
Constance,
Germany
Tetric EvoCeram
Bulk Fill
Ivoclar Vivadent,
Schaan,
Liechtenstein

Universal restorative

A3

N116619

Low shrink posterior

restorative

2.5

A3

N138530

Posterior bulk ll owable base

Universal

100128

Low stress owable composite

Universal

010030

Posterior restorative

Universal

1007001127

Moldable posterior composite

for bulk-lling technique

IVA
(reddish universal
shade)

IDS

1.5 mm, 2.0 mm, 2.5 mm, 3.0 mm, 3.5 mm, 4.0 mm, 4.5 mm,
5.0 mm, 6.0 mm, 7.0 mm, 8.0 mm, 9.0 mm, 10.0 mm, 11.0 mm,
12.0 mm, and 13.0 mm. Programming of the hardness indentation device for dened distances and reproducible placement
of the mold ensured that the VHN measurements were made
along the same axis on each specimen. VHN measurements
were made at a load of 3 g for 15 s. For each of the 12 groups (i.e.
six materials light-cured for either 10 s or 20 s), 22 specimens
were prepared and thus 22 VHN measurements were made at
each of the dened distances.

2.3.

Statistical analysis

In each of the 12 groups, the maximum VHNmax of the VHN values obtained at the dened distances = {0.1, 0.2, 0.5, 1.0, 1.5,
2.0, 2.5, 3.0, 3.5, 4.0, 4.5, 5.0, 6.0, 7.0, 8.0, 9.0, 10.0, 11.0, 12.0, 13.0}
was identied for each of the 22 specimens. For each group,
max

the median VHN
of the 22 VHNmax values as well as the
ISO

of the six DISO values was derived. Then the VHN

median D
ISO
at the biggest depth that was equal to or smaller
value VHN
ISO was determined (Fig. 2). To assess which percentage
than D

Fig. 1 Specimen preparation for depth of cure determination by Vickers hardness measurements. A = stainless steel mold
with semicircular notch, B = stainless steel shell, C = semicircular opening for light-curing, and D = mold including the resin
composite specimen.

524

[3.04,4.24]
[1.83,2.57]
[3.49,4.86]
[2.73,3.28]
[2.84,4.48]
[8.15,67.26]
3.57
2.09
3.94
3.04
3.71
38.25
[1.09,1.74]
[1.53,2.51]
[2.31,2.71]
[3.80,4.16]
[2.87,4.60]
[0.10,1.50]
1
0
3
1
0
5
1.5
2.0
2.5
4.0
3.5
0.2
[52.16,61.27]
[76.35,91.77]
[40.43,50.30]
[34.58,36.88]
[28.50,34.71]
[36.75,52.73]
60.7
83.3
46.5
36.0
32.5
51.5
[61.83,73.60]
[52.01,59.10]
[15.23,19.94]
[12.61,13.49]
[64.81,75.15]
[35.03,65.88]
68.50
55.95
17.65
13.05
70.10
51.95
[2.60,2.74]
[2.05,2.13]
[4.89,4.97]
[6.02,6.12]
[6.41,6.60]
[3.73,3.89]
Filtek Supreme Plus
Filtek Silorane
Surel SDR
Venus Bulk Fill
Quixl
Tetric EvoCeram Bulk Fill

2.68
2.09
4.93
6.08
6.49
3.83

95% CI

[3.91,6.57]
[1.07,2.06]
[1.03,6.89]
[3.16,3.25]
[4.58,11.44]
[3.32,33.20]
4.72
1.76
4.33
3.21
5.72
4.43

Median
95% CI

[0.54,1.26]
[1.87,2.16]
[1.55,2.54]
[2.98,3.02]
[1.07,2.35]
[0.23,1.77]
0
0
3
2
0
9
1.0
2.0
2.0
3.0
2.0
1.5
[51.57,65.33]
[83.05,91.10]
[27.32,46.01]
[42.21,47.83]
[23.62,30.21]
[29.32,50.15]
62.7
84.7
44.2
46.0
25.6
40.8
[51.74,65.10]
[54.40,61.08]
[14.34,16.72]
[8.84,10.00]
[57.57,67.10]
[39.87,62.19]
59.45
58.40
15.60
9.45
62.20
48.55
[2.32,2.40]
[1.70,1.80]
[4.28,4.37]
[4.76,4.86]
[5.69,5.76]
[3.29,3.35]
2.36
1.76
4.33
4.81
5.72
3.32

Nmiss
Median
95% CI
Median
95% CI
Median

fnew n = 22
Dnew (mm) n = 22
pISO (%) n = 6
VHNmax n = 22

20 s

max


ISO varied between 25.6%
attained at D
age pISO of VHN
and 84.7%, with the bulk ll materials retaining less than
max

50% of their VHN
whereas Filtek Supreme Plus retained
around 60% and Filtek Silorane retained slightly more than
max

80% of their VHN
. The biggest depth Dnew above which

Filtek Supreme Plus

Filtek Silorane
Surel SDR
Venus Bulk Fill
Quixl
Tetric EvoCeram Bulk Fill

of VHNmax varied between 9.45 VHN and 70.10 VHN, with

the two owable bulk ll materials (Surel SDR and Venus
max

. The percentBulk Fill) yielding the markedly lowest VHN

10 s

The Vickers hardness proles for the 22 individual specimens

of each of the six resin materials and the two light-curing
times are shown in Figs. 3 and 4. In Table 2 medians and
95% bootstrap condence intervals for the medians are given
for DISO , VHNmax , pISO , Dnew and fnew for each of the six resin
composites and the two light-curing times.
ISO of DISO for the six resin composites varThe median D
ied between 1.76 and 6.49 mm, with the bulk ll materials
ISO than the control materials (Filgenerally yielding higher D
max

tek Supreme Plus and Filtek Silorane). The median VHN

95% CI

Results

Median

3.

DISO (mm) n = 6

max


ISO , VHNISO was divided by
pISO of VHN
was attained at D
max
new

. The biggest depth D
, above which at least 80% of
VHN
max

VHN
was attained, and the factor fnew , by which the absolute length should be divided in order to arrive at Dnew , was
calculated for each specimen. For certain specimens VHN was
max

never above 80% of VHN
. For these specimens Dnew and
new
f
could not be calculated and the number of such incalculable cases was called Nmiss . For DISO , VHNmax , pISO , Dnew and
fnew medians and 95% bootstrap condence intervals for the
medians were determined for each of the 12 groups.
All calculations were performed with R version 2.13.0
(The R Foundation for Statistical Computing, Vienna, Austria;
www.R-project.org), using descriptive methods.

Resin composite

attained).

Light-curing

Fig. 2 Schematic depiction of the identication of VHNmax

and VHNISO (the VHN value at the biggest depth that was
ISO ) as well as the calculation of
equal to or smaller than D
max
new

D
(the depth above which at least 80% of VHN
was

Table 2 Median and 95% bootstrap condence interval for DISO (depth of cure determined by the ISO 4049 method), VHNmax (maximum of the VHN values obtained at
max
max


ISO ), Dnew (the biggest depth above which at least 80% of VHN
the dened distances), pISO (percentage of VHN
attained at D
was attained), and fnew (the factor by
new
).
which the absolute length of specimens, as determined by the ISO 4049 method, should be divided in order to arrive at D

d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

525

L of
Fig. 3 Light-curing for 10 s: Vickers hardness proles for each resin composite (n = 22 per resin composite). Medians A
ISO of depth of cure obtained by the ISO 4049 method, and new depth of cure Dnew for each resin
absolute length, D
composite.

max


at least 80% of VHN
was attained varied between 0.2 and
new

ISO for all resin combeing smaller than D

4 mm, with D
posites except Filtek Silorane (Figs. 3 and 4). The factor fnew
by which the absolute length should be divided in order to
arrive at Dnew varied between 1.76 and 38.25, with fnew being
higher than the division factor two of the ISO 4049 method
for all resin composites except Filtek Silorane. Nmiss varied
between 0 and 9 with the high-viscosity bulk ll material Tetric

EvoCeram Bulk Fill displaying the highest number of incalculable cases.

4.

Discussion

This study showed great variation between the six resin composites as regards depth of cure DISO determined by the ISO
4049 method with the bulk ll materials, true to their name,

526

d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

L of
Fig. 4 Light-curing for 20 s: Vickers hardness proles for each resin composite (n = 22 per resin composite). Medians A
ISO of depth of cure obtained by the ISO 4049 method, and new depth of cure Dnew for each resin
absolute length, D
composite.

yielding higher DISO than the two control materials. Possible

explanations for the higher DISO of the bulk ll materials are
more potent initiator systems and higher translucency. Nevertheless, even with a light-curing time as short as 10 s all six
resin composites met the requirement stipulated in the ISO

4049:2000 of a DISO not less than 1.5 mm. ISO 4049:2000 additionally requires that the depth of cure shall be no more than
0.5 mm below the value claimed by the manufacturer when
using the recommended light-curing time. Only one resin
composite, at only one of the two light-curing times, did not

d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

meet this requirement: The manufacturer indicates that Tetric EvoCeram Bulk Fill may be light-cured to a depth of 4 mm
using a light-curing time of 10 s provided that the light power
density is 1000 mW/cm2 . Yielding a DISO of 3.32 mm Tetric
EvoCeram Bulk Fill did not quite obtain the minimum DISO
required of 3.5 mm (i.e. 4.0 mm claimed by the manufacturer
minus 0.5 mm). As regards the inuence of light-curing time,
doubling the time from 10 s to 20 s led to an average increase
in DISO of 17%. This increase is in agreement with the 1623%
previously found as a result of doubling the light-curing time
[21,22].
The six resin composites also varied markedly regarding
Vickers hardness proles. The hardness proles of the four
bulk ll materials were wider than those of the control materials (as evidenced by the stretched-out hardness proles)
indicating that the point at which VHN could not be measured
anymore due to softness occurred at a much bigger depth for
the bulk ll materials. It is noteworthy that this point at which
VHN could not be measured occurred at smaller depth than
L of the hardened resin composite specthe absolute length A
imens determined by the ISO 4049 method (Figs. 3 and 4) for
all resin composites except Filtek Silorane. This discrepancy
may be the result of a limited resolution of the microhardness indentation device at relatively low surface hardnesses.
The hardness proles of the two owable bulk ll materials
were atter than those of the other materials indicating that
max

VHN
of the two owable bulk ll materials was markedly
lower. The inferior hardness can be explained by a lower ller
content necessary for obtaining the reduced viscosity. Furthermore, regardless of resin composite and light-curing time,
most hardness proles showed that VHNmax was not reached
at the very rst measuring depth of 0.1 mm but rather in
subsurface areas at a depth of 0.2 mm to 1.0 mm. This phenomenon has been previously described [23].
max

ISO was
The percentage of VHN
attained at the depth D
ISO
ISO
assessed and expressed as p . Whereas p
was above 80%
for one of the control materials (Filtek Silorane), pISO was much
lower particularly for the bulk ll materials, which showed in
the median a pISO of only 40%, reecting the different forms
of the Vickers hardness proles.
Numerous studies have dened depth of cure based on
hardness measurements performed on the top and bottom
surface of a light-cured resin composite specimen. The hardness values obtained were used to calculate a bottom/top
hardness ratio, and a ratio above 80% has often been used
as a minimum acceptable threshold value [14,24]. Analogically, in the present study a threshold of 80% was used in
order to determine a depth of cure based on the Vickers hardness measurements: Thus, Dnew was dened as the depth
max

was obtained. Dnew varied
at which at least 80% of VHN
between 1 and 4 mm. There was, however, one exception in
that Tetric EvoCeram Bulk Fill yielded a Dnew of only 0.2 mm
when light-cured for 20 s. The reason for this very low value
is mainly that the hardness of a majority of Tetric EvoCeram
Bulk Fill specimens dropped drastically after the rst measuring depth (0.1 mm). Except for Filtek Silorane, the Dnew
values were lower than the DISO values indicating that the
ISO 4049 method overestimated the depth of cure, especially
for the bulk ll materials as already evidenced by the pISO
values. This nding is in corroboration with that of Moore

527

and coworkers, who concluded that the ISO 4049 method

overestimated depth of cure compared with Knoop hardness
proles [24].
The factors fnew by which the absolute length as determined by the ISO 4049 method should be divided in order
to arrive at Dnew were, consequently, higher than the factor
2 stipulated in the ISO 4049 method except for Filtek Silorane. For the other resin composites, a division factor of 5 (in
the case of 10 s light-curing) or 4 (20 s light-curing) would be
more accurate. Again, the drastic drop in hardness after the
rst measuring depth of 0.1 mm accounts for the exceptionally high fnew calculated for Tetric EvoCeram Bulk Fill at 20 s
light-curing.
In seven of the 12 groups it happened for certain specimens that none of the VHN values measured at the dened
max

of that group, and
distances were above 80% of the VHN
for these specimens Dnew and fnew could not be calculated.
The number of such incalculable cases Nmiss varied markedly
and was especially high for Tetric EvoCeram Bulk Fill, which
led to a biased estimation of Dnew and fnew . On one hand when
light-cured for 10 s, nine specimens of Tetric EvoCeram Bulk
max

Fill showed no VHN value above 80% of VHN
and thus, Dnew
new
and f
remained similar to those of the other resin composites. On the other hand when light-cured for 20 s, for many
max

,
specimens only the rst VHN value was above 80% of VHN
leading to very low Dnew and thus very high fnew . It must be
mentioned, however, that the Tetric EvoCeram Bulk Fill used in
the present study was a preliminary material not yet intended
for in vivo use and not yet on the market at the time of the
measurements.
A recent study investigated depth of cure using numerous
measurement techniques and the authors concluded that not
only depth of cure measured similarly to the ISO 4049 method
but also Vickers hardness proles overestimated depth of cure
[25]. This implies that in the present study hardness proles
and the resultant Dnew also overestimated depth of cure. However, it should be noted that depth of cure determined on the
basis of hardness proles was calculated differently in the two
studies: In the previous study, depth of cure was dened as the
depth at which at least 80% of the hardness measured on the
upper surface of the resin composite was obtained whereas in
the present study, depth of cure Dnew was dened as the depth
at which at least 80% of the maximum hardness (VHNmax ) was
obtained. As VHNmax was most often obtained in subsurface
areas and not at the upper surface, it is uncertain whether or
to what extent Dnew overestimated depth of cure.

5.

Conclusion

The present study found that for bulk ll materials the ISO
4049 method overestimated depth of cure compared to the
determination by Vickers hardness estimations of the degree
of conversion.

Conicts of interest
The authors declare no conicts of interest, real or perceived,
nancial or nonnancial.

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d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) 521528

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