The release of fluorideand other

chemical species from a glass-ionomer

cement
AD.Wilson,
D.M.Groffman
Laboratory of the Government Chemist, Department
London SE1 8x/. UK

of Trade and Industry, Cornwall House, Waterloo Road,

A.T.Kuhn
Faculty of Science and Technology, Harrow College of Higher Education, Northwick Park Harrow, HA1 3TP, UK
(Received 18 June 1984; revised 15 April 1985)

The elution of fluoride, sodium and silica from a glass-ionomer cement was studied for 598 days. It was
found that these species were still being released when the experiments were concluded, however, the rate
of release was much diminished. The release of fluoride, sodium and silica was incongruent. Only fluoride
associated with sodium appeared to be available for release.
Keywords: Dental materials, fluoride, cement, glass-ionomer

Glass-ionomer cement is used in dentistry both for filling

cavities and cementing fixed prostheses. It is translucent,
with optical properties similar to enamel, adheres both to
enamel and dentine and releases fluoride. This latter
property is important for it confers caries resistance on
adjacent tooth material. Early studies carried out over a
period of a few weeks indicated that although the release
rate decreased with time, fluoride would continue to be
released indefinitely. However, more recently Causton*
threw doubts on this assumption and reported that the
release of fluoride ceased after a few months. If this were so,
then the caries resistant properties of glass-ionomer cement
would be of limited duration. A study of Kuhn, Winter and
Davies3 gave a contrary indication to that of Causton*. The
present study sought to clarify the situation by carrying out
studies on fluoride release over a prolonged period of time
i.e. some 20 mnth.

EXPERIMENTAL
The glass-ionomer cement, Chembond, was used in this
study. This material comes as a two-component
pack,
consisting of a powdered fluorine-containing alumino-silicate
glass and a concentrated solution of an acidic polyelectrolyte.
The composition of the glass by weight is: 12.5% Si, 15.6%
Al, 17.7% Ca, 1.8% Na, 31 .O% 0, 18.9% F, 2.5% P; and of
the liquid also by weight: 47.5% poly(acrylic/itaconic acid),
5.0% tartaric acid in water.
The cement was prepared by mixing these two
components together in the ratio 2.6 : 1 .O (by mass) at 23C
and 50% relative humidity. The freshly mixed paste was
cast, using a suitable mould, either as a disc (20 mm diam.
0 1985

x 1.5 mm thick) or as a cylinder (12 mm high X 6 mm diam.).

A platinum wire was inserted in each specimen before
curing. After curing in a sealed mould for 60 min at 37C,
each specimen was removed from the mould, trimmed and
weighed. Four samples of each type of test specimen were
prepared. Each specimen, suspended by the platinum wire,
was placed in 50 ml of distilled water at 37C. The water
was changed periodically during the course of the study. The
water changes were made at 15,45, 105,225
min; 24,48
and 72 h timed from the initial immersion of the cement disc.
Thereafter the water was changed at weekly intervals until
the study was concluded. All the aqueous extracts were
retained and analysed for sodium and silica using Induction
Coupled Plasma Spectrometry. Fluoride was determined
with a fluoride electrode using a TISAB (Total Ionic Strength
Adjustment Buffer). (This reagent is: 0.1% trans-1,2diaminocyclohexane-N,N,N
acid, 8.2%
acetic acid,
5.8% sodium chloride, 0.5% sodium hydroxide adjusted to
pH 5.8 with acetic acid).
Mean values of four results (for both discs and cylinders)
were recorded.

RESULTS AND DISCUSSION

Experimental results can be conveniently expressed as
cumulative log-log plots of fluoride, sodium and silica
against time (Figures 7 and 2). These plots closely approximate to a straight line. Discs which have a greater surface
area than cylinders, release proportionally greater amounts
of fluoride, sodium and silica into solution. Contrary to the
findings of Causton*, fluoride was still being released after
598 d (the period of the experiment) although at a diminished

Butterworth Et Co (Publishers) Ltd. 0142-9612/85/060431-03$03.00

Biomaterials

1985, Vol 6 November

431

Release of F: AD. Wilson et al.

rate. The release of fluoride, sodium and silica from the

cement specimens is incongruent. Although there are only
minor amounts of Na present in the cement (1.3%) compared
with major amounts of F (13.65%)
and Si02 (19.3%) the
amount of sodium eluted is about twice that of both fluoride
and silica Results show that a considerable proportion of the
sodium present in the cement is released during the period
of study. This point is illustrated in Tab/e 1.
Since sodium is the only cation eluted in major
amounts clearly in order to preserve elactroneutrality,
equivalent amounts of fluoride must be released. Thus, the
release of sodium controls that of fluoride. Fluoride associated
with cations otherthan sodium appears to be unavailable for
release. A reasonable inference to be drawn from these
results is that between a third and a half of the available
fluoride is released. thus even after 20 mnth there is still a

300(

2ooC
E
ou
L
1ooc

200

400
Time

600

(d)

5ooc

;
P
I
1.0

IO

100

10

Time (d)
Figure 1 Log-log plot of the cumulative leach of F, Ne and SiO, from glassionomer cement discs against time at 37C: 0. Na; X F; 0. SiO,.

200

400
Time

e 0

(d)

3ooc

c
8
w 2ooc
0
Z
1.0

10

100

1c

Time Cd)
Figure 2 Log-log plot of the cumuletive leach of F, Ne and SiO, from glassionomar cylinders against time at 37C: q. Na; X F; 0, SiO,

Table 1

432

Percentage element eked

from cement specimens (598 dj

Element

Discs

Cylinders

Na
F
Si02

47.0
2.3
2.2

32.0
1.1
1.1

Biomaterials

1985, Vol6 November

1000

i
C
Time

(d)

Figure 3 ~plication of Equation I to release of 3 separste specks, from a

glass-ionomer cement monitored simu~affeoos~ over 598 d. (a) F; (b) Ne:
(c) SiO,.

Release of E RD. Wilson et al.

reservoir of available fluoride. It would seem, ultimately, that

when all the sodium in the cement is eluted, some 4.5% of
the total fluoride present will be released. Clearly, if a greater
fluoride release is demanded then ionomer cements will
have to be formulated with glasses containing greater
amounts of sodium.
The leaching of soluble material from glass-ionomer
and dental silicate cements has been reviewed in detail

Tab/e 2
Species

y = const + at + bT

where y is the total cumulative amount of a species released

in time t and a and bare constants. The goodness-of-fit for F,
Na and SiOz: released from discs and cylinders is good
(Table 2, Figure 3).

Goodness-of-fit (%)

From cement discs

F
Na
SiO,

- 84.2
- 62.9
-220.9

From cement cylinders

F
- 24.8
Na
- 21.2
SiO,
- 64.6

+196.5
+552.5
i-273.6

- 2.317
-11.759
- 2.944

99.92
99.92
99.62

+ 64.3
+219.5
+ 96.6

99.52
99.94
99.96

3
0.754
3.817
1.136

(1)

REFERENCES

Elution values for constants in Equation 1

Constant

elsewhere4, where it has been shown that the release with

time can be described by the equation:

Wilson, A.D. and Presser. H.J., Aluminosllicate dental cements, in

Biocompatibility of Dental Materials: Biocompatibility of Dental
Restorative Materials (Eds DC. Smith and D.F. Williams), Vol. 3.
CRC Press, Boca Raton, 1982, Ch. 3
Causton, B.E.. The physico-mechanical consequences of exposing
glass-ionomer cements to water during setting, Biomateriak 198 1,
2, 112-115
Kuhn, A.T., Winter, G.B. and Davies, EM., Dissolution and fluoride
release from silicate and glass-ionomer cement, J. Dent. Res. 1982,
6, 555 (IADA, Abs. no. 173).
Kuhn. A.T. and Wilson, A.D.. The dissolution mechanisms of silicate
and glass-ionomer cements, Biomaterials

Biomaterials

1985,

6, 378-382

1985. Vol6 November

433