Effect of mixing methods on the physical properties

of dental stones

Shereen S. Azer *, Ronald E. Kerby, Lisa A. Knobloch

Division of Restorative and Prosthetic Dentistry, The Ohio State University College of Dentistry, Columbus, OH, USA
1. Introduction
Dental casts and die materials, especially for xed prostho-
dontic procedures, are required to accurately reproduce the
impressions they are made from, providing all the ne details,
in addition to being dimensionally stable and resistant to
abrasion.
1,2
Several materials that closely fulll these requirements
have been used to fabricate dies. Among these products are
dental stone, epoxy resin, as well as dies electroplated with
metals like copper and silver.
36
Additionally, a blend of stone
and investment material has been proposed to fabricate
refractory dies.
7
Improved dental stones, however, have been by far the
most popular in fabricating working casts and removable dies,
because of their reasonable cost, ease of manipulation, and
ability to produce consistent results, especially high strength/
high expansion (ADA type V) stone.
2,8,9
These products are
commonly mixed either by hand or mechanically under
vacuum. Recently, a new type V stone product, HandiMix
j our na l of d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4
a r t i c l e i n f o
Article history:
Received 13 February 2008
Received in revised form
12 May 2008
Accepted 13 May 2008
Keywords:
HandiMix
Dental stone
Gypsum
Compressive strength
Diametral tensile strength
Setting time
Setting expansion
Surface porosity
Microhardness
Hand-mixing
Vacuum-mixing
Shake-mixing
a b s t r a c t
Objectives: This in vitro comparative study evaluated the effect of different stone mixing
methods on material properties of four dental stones. Two ADA type IV stones (Silky-Rock
and Snap-Stone), one type V high expansion stone (Die Keen), and one recently introduced
type V specialty stone (HandiMix) were chosen for this study.
Methods: Forty cylindrical specimens (25 mm 12.5 mm) were cast for each of the nine
stone sub-groups and bench dried at 23 2 8C for 1 and 24 h. Specimens were then tested in
an Instron in tensile and compression modes at crosshead speeds of 0.5 and 1.0 mm/min,
respectively. Four rectangular-shaped specimens (30 mm 15 mm 15 mm) of each stone
type were cast and bench dried for 48 h. Knoop microhardness measurements were
obtained from dened areas on each specimen for surface hardness testing using 200 g
load and 20 s dwell time. A 12.6 mm
2
area was then delimited in the center of two sides of
each specimen and photographed under low power magnication (40). The average pore
number per area was then determined for each specimen for surface porosity testing. The
setting time and setting expansion for each stone type was recorded as well.
Results: ANOVA (P < 0.001) and RyanEinotGabrielWelsh test (P < 0.05) showed signicant
differences between diametral tensile strengths and pore numbers for both stone types and
mixing methods.
Conclusion: Within the limitations of this study, the newly introduced mixing method did
not appear to have an effect on the physical properties of HandiMix stone.
# 2008 Elsevier Ltd. All rights reserved.

Presented at the 85th General Session of the IADR, 2124 March 2007, New Orleans, LA.
* Corresponding author at: Division of Restorative and Prosthetic Dentistry, The Ohio State University College of Dentistry, 305 West 12th
Avenue, #191, P.O. Box 182357, Columbus, OH 43218-2357, USA. Tel.: +1 614 292 7467; fax: +1 614 292 9422.
E-mail address: azer.1@osu.edu (S.S. Azer).
avai l abl e at www. sci encedi r ect . com
j our nal homepage: www. i nt l . el sevi er heal t h. com/ j our nal s/ j den
0300-5712/$ see front matter # 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2008.05.010
(Whip Mix Corp. Louisville, KY) was introduced to the market.
This material is hand mixed by shaking the pre-weighed
powder and liquid for 20 s in a supplied disposable plastic
container. The stone is then poured into the impression
without the use of additional equipment.
The dimensional accuracy of cast and die materials has
been the subject of several in vitro investigations over the past
decade, with some conicting ndings. Chaffee et al.
10
reported that improved dental stone provided a similar degree
of dimensional accuracy in reproducing a complete arch when
compared to epoxy resin. However, other investigators found
that epoxy resin exhibited considerable shrinkage compare to
gypsumproducts, and suggested that technique modications
were required to obtain castings that would adapt to tooth
preparations if epoxy resin were to be used as die material.
9,11
Heshmati et al.
12
measured the linear expansion of 6 ADA
types IV and V improved dental stone materials and reported
that all stone products showed higher mean linear expansion
values at 120 h compared to 2 h (ADA recommendation).
Other major desirable characteristics of die materials
include surface hardness and abrasion resistance. Ghahre-
mannezhad et al.
13
reported that applying one coat of
cyanoacrylate adhesive as a die hardener to type IV dental
stone increased the surface hardness by 150% and the
abrasion resistance by 48%. In addition, the application of
surface hardeners was shown to create a less porous gypsum
surface.
8
Other investigators however, found that die hard-
eners reduced the surface hardness of gypsum die stones.
14
Furthermore, no signicant difference concerning surface
abrasion and wear resistance was found when conventional
type IV dental stone was compared to resin-impregnated type
IV stone.
15
The compressive and tensile strengths have been the most
common laboratory testing modalities to characterize
mechanical and physical properties of dental stone.
16
Jrgen-
sen and Kono
17
showed that vacuum mixing increased the
compressive strength of dental stone by 20%owing to reduced
gypsum porosity. Some authors reported that the diametral
tensile strengthof type IVstone increasedwhenallowedto dry
in a microwave oven compared to bench top,
18
whereas,
others found that the microwave drying method reduced the
compressive strength of type IV stone.
19
The aim of this in vitro study was to evaluate the inuence
of the various mixing techniques on some physical properties
of dental stone, as well as to compare the newly introduced
HandiMix stone to three other commercially available dental
stones. The null hypothesis was that the physical properties of
dental stone would not be affected by the mixing method
utilized.
2. Materials and methods
Whip Mix Corporation, Louisville, KY 40209, USA and Heraeus
Kulzer, Inc., Armonk, NY 10504, USA supplied the four stone
materials used in this study. Material testing and evaluation
were done according to the American National Standards
Institute/American Dental Association (ANSI/ADA) standards,
specication #25 for dental gypsum products.
20
The materials
were divided into nine groups according to the method of
mixing (Table 1). HandiMix is a new dental stone product that
has been recently introduced to the market. This material is
handmixedby shaking the suppliedpre-measuredpowder and
liquid in a special disposable plastic container for 20 s. The fast
set stone can be separated from the impression after 10 min.
2.1. Compressive and diametral tensile strength testing
For each of the nine study groups, 40 stone cylindrical
specimens (25.0 mm in length and 12.5 mm in diameter)
16
were fabricated for a total of 360 cylinders. All materials were
mixed by the same investigator for standardization purposes,
and poured in a special split-metal mold to obtain the desired
dimensions. Additionally, HandiMix stone was shake-mixed
for 20 s according to the manufacturers directions.
2.1.1. Compressive strength
For each stone group, 20 cylinders were tested in compression
in a Universal Testing Machine (Instron 4204, Canton, MA) in
open air under 1000 kg (10 kN) load at 1.0 mm/min crosshead
speeduntil fracture. Tencylinders were testedafter 1 h, and 10
after 24 h from the setting time. Compressive strength testing
was done on the height of the cylinders with moist lter paper
padding 0.5-mm thick placed between the specimens and the
loading platens. Compressive strength (C) values were
calculated by the formula C = P/pr
2
, where P is the load to
failure and r is the specimen radius.
16,18,19
2.1.2. Diametral tensile strength
The same setup for each stone group was used; 20 cylinders
were tested in tension in the Instron Universal Testing
Machine in open air under 1000 kg (10 kN) load at 0.5 mm/
Table 1 Materials used in the study
Material Mixing method Abbreviation Batch # Manufacturer
Die Keen (DK) Vacuum DKV 0606151 Heraeus Kulzer, Inc.
Hand DKH
Silky-Rock (SR) Vacuum SRV 085080602 Whip Mix Corp.
Hand SRH
Snap-Stone (SS) Vacuum SSV 062060503
Hand SSH
HandiMix (HM) Vacuum HMV P: 21070601 L: 06131 AF
Hand HMH
Shake HMS
j o ur na l o f d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 737
min crosshead speed until fracture. Again, 10 cylinders were
tested after 1 h, and 10 after 24 h from the setting time.
Diametral compressive strength testing was done on the
diameter of the cylinders with moist lter paper padding 0.5-
mm thick placed between the specimens and the loading
platens. Diametral tensile strength (DTS) values were calcu-
lated by the formula DTS = 2P/pdt, where P is the fracture load,
d is the specimen diameter, and t is the thickness or height of
the specimen.
16,18,19
2.2. Surface porosity and microhardness testing
Four rectangular stone block specimens
(30 mm 15 mm 15 mm) were poured for each of the nine
study groups. The blocks were poured into specially designed
silicone molds with the desired dimensions tted on a glass
base. The specimens were allowed to bench-set for 48 h before
testing.
2.2.1. Surface porosity
To resemble the clinical and laboratory situation, where
silicone impressions are generally poured instone, the sides of
the stone block specimens formed by contact with the silicone
molds were used for testing. A circular 12.6 mm
2
area (4.0 mm
diameter) in the center of two sides of each rectangular block
specimen was photographed under low power magnication
(40). Within this circular area on each of the printed color
photographs, a 7.5-mm
2
square area was outlined to deter-
mine by counting, the number of pores inside it. The pores
were photographed and counted by the same investigator for
standardization purposes. Two readings were obtained for
each of the four-stone specimens tested, and were then
averaged to obtain the mean surface porosity count for each
stone group.
2.2.2. Microhardness
Knoop microhardness test was performed using a hardness
tester (M-400, Leco Corp., St. Joseph, MI) equipped with a
Knoop diamond indenter, in accordance with ADA specica-
tion #25 for dental gypsum products.
20
Eight indentations
were obtained for each stone specimen from two surface
locations using 200 g (2 N) load and 20 s dwell time. For each
of the nine-stone groups tested, 32 indentations were
measured, and the average hardness for each group was
calculated.
2.3. Setting time and setting expansion testing
2.3.1. Setting time
For each of the nine study groups, three stone specimens were
poured to estimate the setting time using a standard Vicat
apparatus in accordance with ADA specication #25.
20
The
mean setting time was calculated for each group.
2.3.2. Setting expansion
Evaluation of setting expansion was conducted in accordance
with ADA specication #25.
20
Three specimens were poured
from each stone study group into a 908 V-shaped expansion
device which was lined with rubber dam (Hygienic Dental
Dam; Coltene/Whaledent, Mahwah, NJ) and attached to a
0.01 mm dial caliber (Mitutoyo, Japan). The readings were
averaged for each stone group.
2.4. Statistical analysis
Descriptive statistical analysis was performedfor the collected
data including the meanandstandarddeviationfor eachstone
group using SAS statistical program (version 8.0, SAS Institute
Inc., Cary, NC). Repeated measures analysis of variance
(ANOVA) was used for the differences in means and standard
deviations between the nine-stone groups. The repeated
measures were the mixing methods. The level of signicance
was set at a = 0.05. The RyanEinotGabrielWelsch multiple
range test for each testing parameter was conducted to
evaluate signicant differences between groups.
3. Results
Test results are presented in bar charts representing the
repeated measures analysis of variance (ANOVA) with mean
+1 standard deviation, together with the RyanEinotGabriel
Welsch (REGW) multiple range test analysis. ANOVA (P < .001)
and REGW (P < .05) indicated signicant differences between
the means.
3.1. Compressive and diametral tensile strengths
The mean compressive strengths in MPa for the stone groups
are presented in Fig. 1 and Table 2. The 24-h compressive
strength values of the different stone groups did not showany
signicant difference between vacuum-mixing and hand-
mixing methods. However, within the HandiMix stone sub-
group, the vacuum-mixing method showed a signicantly
higher 24-h compressive strength compared to hand-mixing
and shake-mixing methods for that particular material. This
nding was statistically comparable to the 24-h compressive
strength values of Die Keen and Snap-Stone, and signicantly
higher than Silky Rock (Fig. 1).
The 24-h compressive strength values resulting from
vacuum mixing of the stone groups were signicantly higher
than the 1-h values except for Die Keen and Silky Rock,
which were not signicantly different (Fig. 1). On the other
hand, the 24-h compressive strength values resulting from
hand-mixing as well as shake-mixing for HandiMix stone
were not signicantly different from the 1-h values of the
other stones except for Die Keen and Snap-Stone; which
exhibited a signicantly higher 24-h compressive strength
compared to 1-h. However, these values were not signi-
cantly different from those obtained after 24-h vacuum
mixing (Fig. 1).
Regardless of the mixing method utilized, only Die Keen
and Snap-Stone showed signicantly higher 24-h diametral
tensile strength values expressed in MPa compared to 1-h
(Fig. 2). The hand-mixed Die Keen group exhibited the highest
mean 24-h diametral tensile strengthof all stones, followed by
the vacuum-mixed. Both groups were signicantly stronger
than all other stone groups investigated.
No statistically signicant differences were found between
1- and 24-h in compressive or diametral tensile strength
j our na l of d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 738
values for Silky Rock stone regardless of the mixing method
used (Figs. 1 and 2).
The newlyintroducedshake methodof mixingfor HandiMix
stone showed no signicant difference between 1- and 24-h
regarding diametral tensile strength compared to traditional
vacuum-mixing and hand-mixing methods (Fig. 2). However,
the vacuum-mixing method for that material showed a
signicantly higher 24-h compressive strength (Fig. 1).
3.2. Surface porosity and surface hardness
The mean surface porosity count showed a signicant
difference when the stone mixing methods were compared
(Fig. 3). Vacuum mixing exhibited the least porosity counts
compared to hand mixing except for Snap-Stone (vacuum
mixing for this material is not recommended by the
manufacturer).
Fig. 1 Mean compressive strength in MPa. Similar letters are not statistically significant.
Fig. 2 Mean diametral tensile strength in MPa. Similar letters are not statistically significant.
j o ur na l o f d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 739
Although vacuum mixing for HandiMix stone resulted in
fewer porosity counts, the newly introduced shake mixing
method showed no signicant differences in pore counts
compared to vacuum- or hand-mixing for that material.
Regardless of the mixing method, HandiMix stone exhibited
signicantly reduced surface porosity than hand-mixed Silky
Rock and Snap-Stone (Fig. 3).
Similarly, no signicant differences in surface hardness
(KHN) were found between the different stone study groups,
especially when comparing the shake-mixing method to other
traditional vacuum- and hand-mixing methods (Fig. 4).
3.3. Setting time and setting expansion
There were no signicant differences found between the
different mixing methods regarding the setting time for each
individual stone material (Fig. 5). Die Keen exhibited the
longest setting time of all stones tested and Snap-Stone the
shortest. However, a signicant difference was found between
HandiMix and Die Keen (type V stones) regarding setting
expansion. The hand-mixing method for Die Keen stone
showed a signicantly higher expansion mean than the
vacuum-mixing method. Additionally, both mixing methods
for Die Keen showed signicantly higher setting expansion
means compared to all the other stone groups (Fig. 6).
HandiMix stone, regardless of the mixing method, showed
no signicant differences in setting expansion compared to
type IV stones (Silky Rock and Snap-Stone).
4. Discussion
The null hypothesis in this study (that the physical properties
of dental stones would not be affected by the mixing method
utilized) was accepted. The present investigation was
designed to evaluate a newly introduced method for mixing
dental stone, which reduces time and equipment involved, by
comparing it to traditional mixing techniques in relation to
some of the physical properties of the resultant stone. And
also to compare the newly introduced dental stone (HandiMix)
to other commercially available stones. It is worthy to note
that the stone materials used in this study meet the
requirement values set forth by the ANSI/ADA specication
#25 for gypsum products.
It has been reported that for practical purposes, stone casts
should be separated from impressions after approximately
Table 2 Mean compressive and diametral tensile strengths in MPa of the stone materials for the various mixing methods
Material Mixing method Test Time (h) N Mean S.D.
Die Keen (DK) Vacuum Compressive 1 10 43.5 7.4
24 10 48.4 8.8
Diametral tensile 1 10 5.3 0.8
24 10 7.1 1.7
Hand Compressive 1 10 32.8 6.0
24 10 52.9 11.1
Diametral tensile 1 10 4.6 0.6
24 10 8.7 1.0
Silky-Rock (SR) Vacuum Compressive 1 10 34.4 2.1
24 10 37.8 3.1
Diametral tensile 1 10 4.0 0.3
24 10 4.2 0.7
Hand Compressive 1 10 31.0 4.0
24 10 33.5 5.9
Diametral tensile 1 10 4.4 0.4
24 10 3.6 0.4
Snap-Stone (SS) Vacuum Compressive 1 10 32.2 3.4
24 10 45.0 4.6
Diametral tensile 1 10 3.5 0.5
24 10 5.2 1.0
Hand Compressive 1 10 31.8 6.5
24 10 45.5 5.2
Diametral tensile 1 10 3.3 0.5
24 10 5.2 0.9
HandiMix (HM) Vacuum Compressive 1 10 31.9 4.2
24 10 53.1 8.6
Diametral tensile 1 10 4.1 0.5
24 10 3.9 0.5
Hand Compressive 1 10 33.5 3.6
24 10 31.0 4.2
Diametral tensile 1 10 3.8 0.5
24 10 3.3 0.5
Shake Compressive 1 10 36.7 5.1
24 10 32.9 2.7
Diametral tensile 1 10 4.5 0.6
24 10 3.7 0.4
j our na l of d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 740
45 min to 1 h,
21
and that dental stone would reach sufcient
hardness after 24 h.
22
In this investigation, and in accordance
with the compressive strength testing described by Tuncer
et al.
19
, stone specimens were tested in compression and
tension after 1- and 24-h from the start of mixing.
Earlier investigations suggested that vacuum-mixing pro-
vided a denser and more homogeneous stone mix with less
entrapped air compared to hand mixing.
17,21,23
In the present
investigation, however, there was no signicant difference
found in compressive strength values between both methods
after 24-h, except within the HandiMix stone sub-group,
where vacuum mixing showed a higher compressive strength
for this material. In contradiction to previous reports, hand-
mixed Die Keen stone showed the highest diametral tensile
strength after 24-h compared to all other stone groups. These
inconclusive ndings may suggest that the method of mixing
of dental stone might not necessarily affect the strength of the
set stone.
Fig. 3 Mean surface porosity counts.
Fig. 4 Mean Knoop hardness number (KHN). Similar letters are not statistically significant.
j o ur na l o f d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 741
Specimen dimensions for compressive strength testing
were prepared in accordance with ANSI/ADA standards as
well as with previous similar investigations which consis-
tently exhibited 2:1 length to diameter ratio. Some used
cylindrical specimens 40 mm in length 20 mm in dia-
meter,
1820
while others used cylinders of 12 mm in
length 6 mm in diameter
16
or 10 mm in length 5 mm in
diameter.
24
In the present study cylindrical stone specimens
(25 mm in length 12.5 mm in diameter) were prepared.
However, for the diametral tensile strength testing, previous
investigators used varying geometrical specimen designs.
Some used at cylindrical specimens 10 mm in diame-
ter 3 mm in height,
16
while others used cylinders of equal
diameter and height (5 mm 5 mm).
24
In a recent publication
by Hersek et al.
18
the same geometrical design used for
compressive testing was used for diametral tensile strength
testing (40 mm in height 20 mm in diameter). The present
study followed the model set forth by Hersek et al.
18
being the
most recent.
Althoughnot recommended by the manufacturer, and only
for comparison reasons in this investigation, the fast setting
Snap-Stone was vacuum-mixed for 5 s using the Vac-U-Spat
(Whip Mix Corp., Louisville, KY). Winkler et al.
25
conducted the
same technique for 10 s, but in the current study, and after
Fig. 5 Mean setting time in minutes for the various stone study groups. Similar letters are not statistically significant.
Fig. 6 Mean setting expansion for the various stone study groups. Similar letters are not statistically significant.
j our na l of d e nt i s t r y 3 6 ( 2 0 0 8 ) 7 3 6 7 4 4 742
multiple pilot trials, 5 s were found to be the optimum time
limit to vacuum-mix and pour the fast set stone into the split
mold before hardening. Perhaps this short mixing time under
vacuum was not enough to prevent the formation of voids
within the set stone, as evidenced by the large number of
porosities found in that sub-group comparable to the hand
mixing (Fig. 3). However, the surface hardness of this stone
was not statistically weaker than the other stone groups
(Fig. 4). This might be explained by the almost complete
reaction of the fast setting stone within the early minutes, as
seen by Winkler et al.,
25
who found that the microstructure of
Snap-Stone, as observed by SEM at 10 min, was essentially
unchanged after 24 h. Additionally, in the present investiga-
tion, hardness testing was conducted after 48 h. Previous
investigators reported that after 48 h air dried stone products
exhibited their greatest surface hardness.
26
The results of the
present study probably conrm such reported ndings, as
none of the stone mixing methods showed statistically
signicant difference between the mean KHN values of the
tested stone groups (Fig. 4).
Furthermore, the various stone mixing methods, in this
study, did not seem to affect the setting time or setting
expansion of each of the tested dental stones. Interestingly,
vacuum-mixed Snap-Stone (not recommended by the man-
ufacturer) was not statistically different from the hand-mixed
product.
The introduction of newand innovative mixing techniques
for restorative and prosthetic dental materials is certainly an
encouraged effort, especially if the time involved is reduced
and procedures become more efcient. The limitations of this
study included comparing only four dental stones, as well as
comparing a mixing method that was designed by the
manufacturer for only one type. The authors attempted to
standardize the study as far as was applicable in order to
obtain meaningful statistical results.
5. Conclusions
This investigation evaluated the effect of various stone mixing
techniques on the physical properties of the newly introduced
material, HandiMix, as well as other type IV and V dental
stones. Within the limitations of this study, the following
conclusions are drawn:
1 Mixing methods did not appear to have signicant effect on
the physical properties of dental stone.
2 Shake-mixing for HandiMix stone proved to be an accep-
table alternative to traditional mixing methods, without
affecting the physical properties of the stone.
3 HandiMix specialty stone was not statistically different inits
physical properties from ADA Type IV stones.
Acknowledgements
The authors thank Whip Mix Corporation, Louisville, KY and
Heraeus Kulzer, Inc., Armonk, NY, for supplying the materials
used in this study.
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