Dental Research

Effects of acid-etching solutions on hnman enamel and dentin

Marco Franchi*/Lorenzo Breschi**
Nine noncarioiis human molars were exiracled and stored in saline solution. Three standard
ocdiisal caviiies with beveled enamel margins were prepared on each tooth andetchedwith the
etching solutions of three dminai adhesive systems.- ( 1 ) 37% plmsphoric acid solution. (2)
4.3% oxalic add and 2.6% alumium salts solution, and (3) 10% maleic add solution. Scanning
electron microscopic analysis revealed that all the etching .solutions affected the enamel
surface morphology. The solution of oxalic acid and aluminum salts removed primarily the
prism core material and partially the periphery of the prisms, but did not affect the nonbeveled
enamel surface. Phosphoric and maleic adds removed both prism core tnateriah and prism
periphery',- these specimens also showed areas in which no prism morphology could be detected.
These two acids also removed apatite crystals from the prism core of the intact enamel surface.
(Quintessence Int 1995.-26:431-435.)

Introduction

The acid-etching technique with phosphoric acid,

introduced by Buonocore' in 1955, is still used to
create an irregular surface of beveled enamel. This
allows an increase in the cavity surface available for the
retention of resin composites and an improvement in
marginal adaptation of restorations.^'* Moreover, the
benefits of acid etciiing include an increased resistance
to recurrent caries both in enamel and cement.'''"
Three types of etching patterns have been described
by Silverstone et al" after exposure of the enamel
prisms to etching solutions: type I, preferential removal of prism core material, leaving the periphery intact;
type II, preferential removal of periphery core material,
leaving the prism core relatively unaffected; and type
in, a more random etching pattern in which adjacent
areas of the tooth surface correspond to types I and II,
mixed with regions in which the pattern could not be
related to prism morphology.

" Depajtment of Oral Surgery, University of Bologna, School of

Dentistry, Bologna, Italy.
" University of Bologna, School of Dentistry, Bologna, Italy,
Reprint requests: Dr Marco Franchi, via del Triumviralo 9, 40132
Bologna. Italy.

Quintaseefiee4n(wnatWl31

6/1995

Many factors influence the effects of acid etching on

beveled enamel: the acid-etching solution, its concentration, the technique used, and the time of application
arc the parameters subject to greatest investgation.'-"'^
Different etching solutions have recently been tested:
phosphoric acid (solutions between 30% and 50%),
flouridated phosphoric acid, pyruvic acid, citric acid,
maleic acid, oxalic acid, tannic acid, ethylenediaminetetraacetic acid, trichloracetic acid, and polyacrylic
acid,'-'^'*"^' The physical status of the solution is
another important parameter. The gel-type etching
agent seems easier to apply on the enamel surface than
docs the liquid form, and it is reported to produce a
wider and deeper penetration of enamel.^^ The method
of application of the etching agent has also been
investigated to improve clinical success. A continuous
brushing technique may be used to apply an acid
etching gel to obtain a more etched enamel wall and
therefore an improvement in the marginal adaptation
of the resin composite restoration.'^"''' Another factor
that may influence the effects of acid etching and can
reduce microleakage as well is the shape of the beveled
enamel, ^^'^^
In this study, the morphologic aspects of the enamel
surface after treatment with three different acid-etching
agents have been investigated by scanning electron
microscope (SEM).

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Dental Research
Method and materials

Nine noncadous and nonfractured human molars that

were extracted because of periodontal disease were
stored in 0.9% saline solution for 48 hours at 37C.
Three standard occlusal cavities, approximately 2 mm
wide, were prepared in each tooth with a round
diamond (Intensive No. 201 ), in a high-speed handpiece. The enamel margins were then heveled ( 120-to
130-degree cavosurface angle) with a diamond buttjoint bur (Intensive No, 206),
All cavity walls and cavosurface margins were
etched with one of the following solutions in accordance with each manufacturer's instructions: (I) 37%
phosphoric acid solution (Enamel etchant of Scotchbond 2. 3M Dental) for 30 seconds; (2) 4.3% oxalic
acid and 2.6% aluminum salts solution (Conditioning
solution of Gluma 2000, Bayer Dental) for 30
seconds, (3) \()% maleic aeid solution (Enamel
etchant of Scotchbond MP, 3M Dental) for 15
seconds.
To obtain comparable results, one of three acidetching agents was applied to one of three cavities in
each tooth. This procedure prevented factors such as
differences in tooth age or rates of tissue calcification
from affecting results. After the application of the
acid-etching solutions, all the cavities were rinsed with
water and dried with compressed air.
All the specimens were air dehydrated, positioned
on stubs, and coated (Edwards 150A Sputter Coater)
for 120 seconds at 30 mA with a gold-palladium
coating. The SEM observations (Philips 515) were
carried out at voltages ranging from 5.9 to 10.4 kV. The
picmres of enamel and dentin selected are representative of the pattern that was most often observed on the
specimens.
Results

All the acid-etching solutions affected both the enamel

and the dentinal surface: enamel prism morphology
and dentinal tubule orifices were clearly detectable.
The beveled enamel surface etched with the three
different acid solutions showed (I) areas with preferential removal of prism core material (type 1), (2)
areas with dissolution of the periphery of the prisms
(type II), and (3) areas with amorphous appearances
(type III). No evident morphologie differences were
observed in the beveled enamel surfaces treated with
the three different acid-etching solutions (Figs 1 to 3).
Type I and type il patterns were observed in areas
where the prisms were accidentally cut longitudinally
(Figs 4 to 6).

432

The intact enamel surface etched with the three acid

solutions showed different results. The 37% phosphoric acid removed the apatite crystals from the prism
core thoroughly, leaving a very rough enamel surface
(type I pattern) (Fig 7). The 4.3% oxalic acid and 2.6%
aluminum salts solution did not affect the normal
prism morphology (Fig 8). The 10% maleic acid
resulted in only a partial removal of the enamel apatite
crystals (Fig 9).
Each of the three acid-etching solutions had a
different effect on the dentinal walls. In particular, the
31% phosphoric acid solution removed the smear layer
and opened the dentinal tubule orifices, which appeared empty (Fig 10). With the 4.3% oxalic acid and
2.6% aluminum salts solution, about 50% of the
dentinal tubule orifices were filled with smear layer,
while the rest were partially empty (Fig 11). The dentin
treated with the 10% maleic acid solution showed
opened dentin tubule orifices, and coliagen fibrils
were visible inside the tubules (Fig 12).
Discussion
All three acid-etching solutions modified the beveled
enamel surface, forming pores by selective dcalcification. The new porous enamel surface enhances mechanical interlocking by tag penetration of bonding resin
into the enamel.-""'* Researchers have measured the
interaction between different adhesive systems and
resin composites with etched enamel by shear bond
strength tests.'^-'^'^''^'-* The present morphologic
study did not reveal the qualitative differences described by Silverstone et al" among the effects on the
beveled enamel of the three etching solutions. Type I,
type II, and type III etching patterns were observed in
the different specimens. Confirming the present observations, a clinical trial showed maleic acid and
phosphoric acid to have similar results in Class IV and
Class V restorations.^'
Areas where the prisms were longitudinally cut and
treated with the three acid-etching solutions showed
botli type I and type II enamel etching patterns. This
effect demonstrates that, even when an incorrect
enamel bevel is prepared, the modified enamel surface
might offer retention for penetration of the bonding
resin.
The 37% phosphoric acid solution appiied on intact
enamel promoted enamel dissolution with a type I
pattern, the 4.3% oxalic add and 2.6% aluminum salts
solution did not affect the intact enamel surface, and
the 10% maleic acid partially removed prism core
material. Further clinical studies might demonstrate

Quintessence International

Volume 26.

Dental Research

Fig 1 Beveled enamel surface etched with 37% phosphoric acid solution. Silverstone's etcfiing type II pattern is
evident. (Bar = 10 jim.)

Fig 4 Enamel prisms longitudinally cut and etched with

37% phosphoric acid solution. Bar " 0,1 mm,)

Fig 2 Beveled enamel surface elched with 4.3% oxalic

acid and 2.6% aluminum salts solution Silverstone's type III
etching pattern is detectable, (Bar - 10 \im.)

Fig 5 Enamel prisms longitudinally cut and etched with

4.3% oxalic acid and 2,6% aluminum salts solution.
(Bar = 0.1 mm.)

Fig 3 Beveled enamel surtace etched witii 10% maieio

acid solution Silverstone's type 1 etching pattern may be
recognized, (Bar = 10 \im.)

Fig 6 Enamel prisms longitudinally cut and etched vi/ith

10% maleic acid solution. (Bar = 0,1 mm)

Ouintessene&intcrnBtiuiidl

UUlUlfItf ^Number B/1995

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Dental Research

Fig 7 intact enamel surface etched with 37% phosphoric

acid solution. Highly rough enamel surface (type i patlerni is
visible. (Bar = 10 [irn )

Fig 10 Dentinal surface treated with 37% phosphoric acid

solution. The acid has removed the smear layer and opened
the dentinal tubule orifices, which appear empty.
{Bar= 10 |im.)

Fig 8 Intact enamel surface etched with 4.3% oxalic acid

and 2.6% aluminum salts solution. Tliis etching soiution has
not affected the normal prism morphology. (Bar = ID |im.

Fig 11 Dentinai surface treated with 4.3% oxalic acid and

2.6% aluminum salts solution. About 50% of the dentinai
tubule orifices appear to be fiiied with smear layer, while the
rest are partially empty. (Bar = 10 |im.)

Fig 9 Intact enamel surface etched with 10% maleic acid

solution. Only a partial removal of the enamel apatite
crystals is evident. {Bar - 10 [.im.]

Fig 12 Dentinal surface treated with 10% maleic acid

solution. Denfinal tubule orifices are opened, and collagen
fibriis are visible inside the tubules. (Bar = 10 um.)

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Dental Research
that use of these three acid-etching solutions on intact
enamel (as when orthodontic brackets are applied)
could provide different clinical results.
This study also investigated the effect of applying the
three acid-etching solutions on the dentinal cavity
walls, because clinical rpons'*^ have demonstrated
that patients experience no postoperative sensitivity
and no pain after 18 months. The best removal of
dentinal smear layer resulted from the 37% phosphoric
acid treatment; all the dentin tubules orifices appeared
to be completely opened. With the 4.3% oxalic acid
and 2.6% aluminum salts solution, only 50% of the
dentinal tubule orifices were partially free; tlie rest
were covered by the smear layer. Opened dentin tubule
oriftces, with collagen fibrils inside the tubules, were
present in dentinal surface treated with the 10% maleic
acid solution.

Ackuowledgments
The authors thanks Mr Gianfranco Filippini for technical assistance.

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