journal of dentistry 36 (2008) 736–744

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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

article info abstract

Article history: Objectives: This in vitro comparative study evaluated the effect of different stone mixing
Received 13 February 2008 methods on material properties of four dental stones. Two ADA type IV stones (Silky-Rock
Received in revised form and Snap-Stone), one type V high expansion stone (Die Keen), and one recently introduced
12 May 2008 type V specialty stone (HandiMix) were chosen for this study.
Accepted 13 May 2008 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,
Keywords: respectively. Four rectangular-shaped specimens (30 mm  15 mm  15 mm) of each stone
HandiMix type were cast and bench dried for 48 h. Knoop microhardness measurements were
Dental stone obtained from defined areas on each specimen for surface hardness testing using 200 g
Gypsum load and 20 s dwell time. A 12.6 mm2 area was then delimited in the center of two sides of
Compressive strength each specimen and photographed under low power magnification (40). The average pore
Diametral tensile strength number per area was then determined for each specimen for surface porosity testing. The
Setting time setting time and setting expansion for each stone type was recorded as well.
Setting expansion Results: ANOVA (P < 0.001) and Ryan–Einot–Gabriel–Welsh test (P < 0.05) showed significant
Surface porosity differences between diametral tensile strengths and pore numbers for both stone types and
Microhardness mixing methods.
Hand-mixing Conclusion: Within the limitations of this study, the newly introduced mixing method did
Vacuum-mixing not appear to have an effect on the physical properties of HandiMix stone.
Shake-mixing # 2008 Elsevier Ltd. All rights reserved.

1. Introduction metals like copper and silver.3–6 Additionally, a blend of stone

and investment material has been proposed to fabricate
Dental casts and die materials, especially for fixed prostho- refractory dies.7
dontic procedures, are required to accurately reproduce the Improved dental stones, however, have been by far the
impressions they are made from, providing all the fine details, most popular in fabricating working casts and removable dies,
in addition to being dimensionally stable and resistant to because of their reasonable cost, ease of manipulation, and
abrasion.1,2 ability to produce consistent results, especially high strength/
Several materials that closely fulfill these requirements high expansion (ADA type V) stone.2,8,9 These products are
have been used to fabricate dies. Among these products are commonly mixed either by hand or mechanically under
dental stone, epoxy resin, as well as dies electroplated with vacuum. Recently, a new type V stone product, HandiMix

§
Presented at the 85th General Session of the IADR, 21–24 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).
0300-5712/$ – see front matter # 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2008.05.010
 journal of dentistry 36 (2008) 736–744 737

(Whip Mix Corp. Louisville, KY) was introduced to the market. stones. The null hypothesis was that the physical properties of
This material is hand mixed by shaking the pre-weighed dental stone would not be affected by the mixing method
powder and liquid for 20 s in a supplied disposable plastic utilized.
container. The stone is then poured into the impression
without the use of additional equipment.
The dimensional accuracy of cast and die materials has 2. Materials and methods
been the subject of several in vitro investigations over the past
decade, with some conflicting findings. Chaffee et al.10 Whip Mix Corporation, Louisville, KY 40209, USA and Heraeus
reported that improved dental stone provided a similar degree Kulzer, Inc., Armonk, NY 10504, USA supplied the four stone
of dimensional accuracy in reproducing a complete arch when materials used in this study. Material testing and evaluation
compared to epoxy resin. However, other investigators found were done according to the American National Standards
that epoxy resin exhibited considerable shrinkage compare to Institute/American Dental Association (ANSI/ADA) standards,
gypsum products, and suggested that technique modifications specification #25 for dental gypsum products.20 The materials
were required to obtain castings that would adapt to tooth were divided into nine groups according to the method of
preparations if epoxy resin were to be used as die material.9,11 mixing (Table 1). HandiMix is a new dental stone product that
Heshmati et al.12 measured the linear expansion of 6 ADA has been recently introduced to the market. This material is
types IV and V improved dental stone materials and reported hand mixed by shaking the supplied pre-measured powder and
that all stone products showed higher mean linear expansion liquid in a special disposable plastic container for 20 s. The fast
values at 120 h compared to 2 h (ADA recommendation). set stone can be separated from the impression after 10 min.
Other major desirable characteristics of die materials
include surface hardness and abrasion resistance. Ghahre- 2.1. Compressive and diametral tensile strength testing
mannezhad et al.13 reported that applying one coat of
cyanoacrylate adhesive as a die hardener to type IV dental For each of the nine study groups, 40 stone cylindrical
stone increased the surface hardness by 150% and the specimens (25.0 mm in length and 12.5 mm in diameter)16
abrasion resistance by 48%. In addition, the application of were fabricated for a total of 360 cylinders. All materials were
surface hardeners was shown to create a less porous gypsum mixed by the same investigator for standardization purposes,
surface.8 Other investigators however, found that die hard- and poured in a special split-metal mold to obtain the desired
eners reduced the surface hardness of gypsum die stones.14 dimensions. Additionally, HandiMix stone was shake-mixed
Furthermore, no significant difference concerning surface for 20 s according to the manufacturer’s directions.
abrasion and wear resistance was found when conventional
type IV dental stone was compared to resin-impregnated type 2.1.1. Compressive strength
IV stone.15 For each stone group, 20 cylinders were tested in compression
The compressive and tensile strengths have been the most in a Universal Testing Machine (Instron 4204, Canton, MA) in
common laboratory testing modalities to characterize open air under 1000 kg (10 kN) load at 1.0 mm/min crosshead
mechanical and physical properties of dental stone.16 Jørgen- speed until fracture. Ten cylinders were tested after 1 h, and 10
sen and Kono17 showed that vacuum mixing increased the after 24 h from the setting time. Compressive strength testing
compressive strength of dental stone by 20% owing to reduced was done on the height of the cylinders with moist filter paper
gypsum porosity. Some authors reported that the diametral padding 0.5-mm thick placed between the specimens and the
tensile strength of type IV stone increased when allowed to dry loading platens. Compressive strength (C) values were
in a microwave oven compared to bench top,18 whereas, calculated by the formula C = P/pr2, where P is the load to
others found that the microwave drying method reduced the failure and r is the specimen radius.16,18,19
compressive strength of type IV stone.19
The aim of this in vitro study was to evaluate the influence 2.1.2. Diametral tensile strength
of the various mixing techniques on some physical properties The same setup for each stone group was used; 20 cylinders
of dental stone, as well as to compare the newly introduced were tested in tension in the Instron Universal Testing
HandiMix stone to three other commercially available dental 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
738 journal of dentistry 36 (2008) 736–744

min crosshead speed until fracture. Again, 10 cylinders were 0.01 mm dial caliber (Mitutoyo, Japan). The readings were
tested after 1 h, and 10 after 24 h from the setting time. averaged for each stone group.
Diametral compressive strength testing was done on the
diameter of the cylinders with moist filter paper padding 0.5- 2.4. Statistical analysis
mm thick placed between the specimens and the loading
platens. Diametral tensile strength (DTS) values were calcu- Descriptive statistical analysis was performed for the collected
lated by the formula DTS = 2P/pdt, where P is the fracture load, data including the mean and standard deviation for each stone
d is the specimen diameter, and t is the thickness or height of group using SAS statistical program (version 8.0, SAS Institute
the specimen.16,18,19 Inc., Cary, NC). Repeated measures analysis of variance
(ANOVA) was used for the differences in means and standard
2.2. Surface porosity and microhardness testing deviations between the nine-stone groups. The repeated
measures were the mixing methods. The level of significance
Four rectangular stone block specimens was set at a = 0.05. The Ryan–Einot–Gabriel–Welsch multiple
(30 mm  15 mm  15 mm) were poured for each of the nine range test for each testing parameter was conducted to
study groups. The blocks were poured into specially designed evaluate significant differences between groups.
silicone molds with the desired dimensions fitted on a glass
base. The specimens were allowed to bench-set for 48 h before
testing. 3. Results

2.2.1. Surface porosity Test results are presented in bar charts representing the
To resemble the clinical and laboratory situation, where repeated measures analysis of variance (ANOVA) with mean
silicone impressions are generally poured in stone, the sides of +1 standard deviation, together with the Ryan–Einot–Gabriel–
the stone block specimens formed by contact with the silicone Welsch (REGW) multiple range test analysis. ANOVA (P < .001)
molds were used for testing. A circular 12.6 mm2 area (4.0 mm and REGW (P < .05) indicated significant differences between
diameter) in the center of two sides of each rectangular block the means.
specimen was photographed under low power magnification
(40). Within this circular area on each of the printed color 3.1. Compressive and diametral tensile strengths
photographs, a 7.5-mm2 square area was outlined to deter-
mine by counting, the number of pores inside it. The pores The mean compressive strengths in MPa for the stone groups
were photographed and counted by the same investigator for are presented in Fig. 1 and Table 2. The 24-h compressive
standardization purposes. Two readings were obtained for strength values of the different stone groups did not show any
each of the four-stone specimens tested, and were then significant difference between vacuum-mixing and hand-
averaged to obtain the mean surface porosity count for each mixing methods. However, within the HandiMix stone sub-
stone group. group, the vacuum-mixing method showed a significantly
higher 24-h compressive strength compared to hand-mixing
2.2.2. Microhardness and shake-mixing methods for that particular material. This
Knoop microhardness test was performed using a hardness finding was statistically comparable to the 24-h compressive
tester (M-400, Leco Corp., St. Joseph, MI) equipped with a strength values of Die Keen and Snap-Stone, and significantly
Knoop diamond indenter, in accordance with ADA specifica- higher than Silky Rock (Fig. 1).
tion #25 for dental gypsum products.20 Eight indentations The 24-h compressive strength values resulting from
were obtained for each stone specimen from two surface vacuum mixing of the stone groups were significantly higher
locations using 200 g (2 N) load and 20 s dwell time. For each than the 1-h values except for Die Keen and Silky Rock,
of the nine-stone groups tested, 32 indentations were which were not significantly different (Fig. 1). On the other
measured, and the average hardness for each group was hand, the 24-h compressive strength values resulting from
calculated. hand-mixing as well as shake-mixing for HandiMix stone
were not significantly different from the 1-h values of the
2.3. Setting time and setting expansion testing other stones except for Die Keen and Snap-Stone; which
exhibited a significantly higher 24-h compressive strength
2.3.1. Setting time compared to 1-h. However, these values were not signifi-
For each of the nine study groups, three stone specimens were cantly different from those obtained after 24-h vacuum
poured to estimate the setting time using a standard Vicat mixing (Fig. 1).
apparatus in accordance with ADA specification #25.20 The Regardless of the mixing method utilized, only Die Keen
mean setting time was calculated for each group. and Snap-Stone showed significantly higher 24-h diametral
tensile strength values expressed in MPa compared to 1-h
2.3.2. Setting expansion (Fig. 2). The hand-mixed Die Keen group exhibited the highest
Evaluation of setting expansion was conducted in accordance mean 24-h diametral tensile strength of all stones, followed by
with ADA specification #25.20 Three specimens were poured the vacuum-mixed. Both groups were significantly stronger
from each stone study group into a 908 V-shaped expansion than all other stone groups investigated.
device which was lined with rubber dam (Hygienic Dental No statistically significant differences were found between
Dam; Coltene/Whaledent, Mahwah, NJ) and attached to a 1- and 24-h in compressive or diametral tensile strength
 journal of dentistry 36 (2008) 736–744 739

Fig. 1 – Mean compressive strength in MPa. Similar letters are not statistically significant.

values for Silky Rock stone regardless of the mixing method 3.2. Surface porosity and surface hardness
used (Figs. 1 and 2).
The newly introduced shake method of mixing for HandiMix The mean surface porosity count showed a significant
stone showed no significant difference between 1- and 24-h difference when the stone mixing methods were compared
regarding diametral tensile strength compared to traditional (Fig. 3). Vacuum mixing exhibited the least porosity counts
vacuum-mixing and hand-mixing methods (Fig. 2). However, compared to hand mixing except for Snap-Stone (vacuum
the vacuum-mixing method for that material showed a mixing for this material is not recommended by the
significantly higher 24-h compressive strength (Fig. 1). manufacturer).

Fig. 2 – Mean diametral tensile strength in MPa. Similar letters are not statistically significant.
740 journal of dentistry 36 (2008) 736–744

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

Although vacuum mixing for HandiMix stone resulted in for Die Keen showed significantly higher setting expansion
fewer porosity counts, the newly introduced shake mixing means compared to all the other stone groups (Fig. 6).
method showed no significant differences in pore counts HandiMix stone, regardless of the mixing method, showed
compared to vacuum- or hand-mixing for that material. no significant differences in setting expansion compared to
Regardless of the mixing method, HandiMix stone exhibited type IV stones (Silky Rock and Snap-Stone).
significantly reduced surface porosity than hand-mixed Silky
Rock and Snap-Stone (Fig. 3).
Similarly, no significant differences in surface hardness 4. Discussion
(KHN) were found between the different stone study groups,
especially when comparing the shake-mixing method to other The null hypothesis in this study (that the physical properties
traditional vacuum- and hand-mixing methods (Fig. 4). of dental stones would not be affected by the mixing method
utilized) was accepted. The present investigation was
3.3. Setting time and setting expansion designed to evaluate a newly introduced method for mixing
dental stone, which reduces time and equipment involved, by
There were no significant differences found between the comparing it to traditional mixing techniques in relation to
different mixing methods regarding the setting time for each some of the physical properties of the resultant stone. And
individual stone material (Fig. 5). Die Keen exhibited the also to compare the newly introduced dental stone (HandiMix)
longest setting time of all stones tested and Snap-Stone the to other commercially available stones. It is worthy to note
shortest. However, a significant difference was found between that the stone materials used in this study meet the
HandiMix and Die Keen (type V stones) regarding setting requirement values set forth by the ANSI/ADA specification
expansion. The hand-mixing method for Die Keen stone #25 for gypsum products.
showed a significantly higher expansion mean than the It has been reported that for practical purposes, stone casts
vacuum-mixing method. Additionally, both mixing methods should be separated from impressions after approximately
 journal of dentistry 36 (2008) 736–744 741

Fig. 3 – Mean surface porosity counts.

45 min to 1 h,21 and that dental stone would reach sufficient found in compressive strength values between both methods
hardness after 24 h.22 In this investigation, and in accordance after 24-h, except within the HandiMix stone sub-group,
with the compressive strength testing described by Tuncer where vacuum mixing showed a higher compressive strength
et al.19, stone specimens were tested in compression and for this material. In contradiction to previous reports, hand-
tension after 1- and 24-h from the start of mixing. mixed Die Keen stone showed the highest diametral tensile
Earlier investigations suggested that vacuum-mixing pro- strength after 24-h compared to all other stone groups. These
vided a denser and more homogeneous stone mix with less inconclusive findings may suggest that the method of mixing
entrapped air compared to hand mixing.17,21,23 In the present of dental stone might not necessarily affect the strength of the
investigation, however, there was no significant difference set stone.

Fig. 4 – Mean Knoop hardness number (KHN). Similar letters are not statistically significant.
742 journal of dentistry 36 (2008) 736–744

Fig. 5 – Mean setting time in minutes for the various stone study groups. Similar letters are not statistically significant.

Specimen dimensions for compressive strength testing ter  3 mm in height,16 while others used cylinders of equal
were prepared in accordance with ANSI/ADA standards as diameter and height (5 mm  5 mm).24 In a recent publication
well as with previous similar investigations which consis- by Hersek et al.18 the same geometrical design used for
tently exhibited 2:1 length to diameter ratio. Some used compressive testing was used for diametral tensile strength
cylindrical specimens 40 mm in length  20 mm in dia- testing (40 mm in height  20 mm in diameter). The present
meter,18–20 while others used cylinders of 12 mm in study followed the model set forth by Hersek et al.18 being the
length  6 mm in diameter16 or 10 mm in length  5 mm in most recent.
diameter.24 In the present study cylindrical stone specimens Although not recommended by the manufacturer, and only
(25 mm in length  12.5 mm in diameter) were prepared. for comparison reasons in this investigation, the fast setting
However, for the diametral tensile strength testing, previous Snap-Stone was vacuum-mixed for 5 s using the Vac-U-Spat
investigators used varying geometrical specimen designs. (Whip Mix Corp., Louisville, KY). Winkler et al.25 conducted the
Some used flat cylindrical specimens 10 mm in diame- same technique for 10 s, but in the current study, and after

Fig. 6 – Mean setting expansion for the various stone study groups. Similar letters are not statistically significant.
 journal of dentistry 36 (2008) 736–744 743

multiple pilot trials, 5 s were found to be the optimum time references

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 1. Covo LM, Ziebert GJ, Balthazar Y, Christensen LV. Accuracy
within the set stone, as evidenced by the large number of and comparative stability of three removable die systems.
porosities found in that sub-group comparable to the hand Journal of Prosthetic Dentistry 1988;59:314–8.
mixing (Fig. 3). However, the surface hardness of this stone 2. Craig RG. Restorative dental materials. 12th ed. Mosby: St.
Louis; 2006.
was not statistically weaker than the other stone groups
3. Crispin BJ, Watson JF, Bauer JG, Frawley KR. Silver-plated
(Fig. 4). This might be explained by the almost complete dies. Part I. Platability of impression materials. Journal of
reaction of the fast setting stone within the early minutes, as Prosthetic Dentistry 1984;51:631–6.
seen by Winkler et al.,25 who found that the microstructure of 4. Crispin BJ, Watson JF, Frawley KR. Silver-plated dies. Part II.
Snap-Stone, as observed by SEM at 10 min, was essentially Marginal accuracy of cast restorations. Journal of Prosthetic
unchanged after 24 h. Additionally, in the present investiga- Dentistry 1984;51:768–73.
tion, hardness testing was conducted after 48 h. Previous 5. Aiach D, Malone WFP, Sandrik J. Dimensional accuracy
of epoxy resins and their compatibility with
investigators reported that after 48 h air dried stone products
impression materials. Journal of Prosthetic Dentistry
exhibited their greatest surface hardness.26 The results of the 1984;52:500–4.
present study probably confirm such reported findings, as 6. Schäffer H, Dumfahrt H, Gausch K. Distance alterations of
none of the stone mixing methods showed statistically dies in sagittal direction in dependence of the die material.
significant difference between the mean KHN values of the Journal of Prosthetic Dentistry 1989;61:684–8.
tested stone groups (Fig. 4). 7. Lund MR, Shryock EF. Castings made directly to refractory
dies. Journal of Prosthetic Dentistry 1967;18:251–6.
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8. Lindquist TJ, Stanford CM, Knox E. Influence of surface
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vacuum-mixed Snap-Stone (not recommended by the man- 9. Kenyon BJ, Hagge MS, Leknius C, Daniels WC, Weed ST.
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The introduction of new and innovative mixing techniques 10. Chaffee NR, Bailey JH, Sherrard DJ. Dimensional accuracy of
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Complete arch form. Journal of Prosthetic Dentistry
encouraged effort, especially if the time involved is reduced 1997;77:235–8.
and procedures become more efficient. The limitations of this 11. Duke P, Moore BK, Haug SP, Andres CJ. Study of the physical
study included comparing only four dental stones, as well as properties of type IV gypsum, resin-containing, and epoxy
comparing a mixing method that was designed by the die materials. Journal of Prosthetic Dentistry 2000;83:466–73.
manufacturer for only one type. The authors attempted to 12. Heshmati RH, Nagy WW, Wirth CG, Dhuru VB. Delayed
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13. Ghahremannezhad H, Mohamed SE, Stewart G, Weinberg R.
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5. Conclusions 14. Harris PE, Hoyer S, Lindquist TJ, Stanford CM. Alterations of
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17. Jørgensen KD, Kono A. Relationship between the porosity
2 Shake-mixing for HandiMix stone proved to be an accep-
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3 HandiMix specialty stone was not statistically different in its IV dental stones dried in a microwave oven. Journal of
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Revised American National Standards Institute/American
The authors thank Whip Mix Corporation, Louisville, KY and Dental Association Specification No. 25 for dental
Heraeus Kulzer, Inc., Armonk, NY, for supplying the materials gypsum products. Journal of American Dental Association
used in this study. 1981;102:351.
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