ORIGINAL ARTICLE

Bond strength comparison of moisture-

insensitive primers
Shane Schaneveldt, DDS, MCID,a and Timothy F. Foley, DDS, MCIDb
London, Ontario, Canada

The objective of this in vitro bonding study was to evaluate the effectiveness of 2 moisture-insensitive
primers, Assure (Reliance Orthodontic Products, Itasca, Ill) and MIP (3M Unitek, Monrovia, Calif) compared
with a control hydrophobic primer, Transbond XT (3M Unitek). Six groups of 40 premolars were acid etched
and bonded using metal orthodontic brackets with the following in vitro protocols: (1) Transbond XT primer
and adhesive applied to a noncontaminated surface; (2) Assure primer applied after saliva contamination; (3)
MIP primer applied after saliva contamination; (4) Assure primer reapplied after saliva contamination; (5) MIP
reapplied after saliva contamination; and (6) Assure adhesive applied after saliva contamination of the primer.
All bonded specimens were stored in deionized water at 37°C for 30 days and thermocycled for 24 hours
before debonding. Brackets were debonded using a shear-peel load on a testing machine, bond strength
was measured in megapascals, and bond failure was analyzed by using the adhesive remnant index. In vitro
shear-peel bond strengths were acceptable for all groups, and the bond strengths for Assure and MIP were
not significantly affected by saliva contamination. The mean shear-peel bond strength of the control (14.82
MPa) was significantly higher (P ⬍ .001) than the contaminated groups with the exception of MIP group 5
(14.02 MPa). The values of the Assure primer and adhesive were less than the MIP primer and its respective
adhesive; however, the hydrophilic Assure adhesive resin applied to a saliva-contaminated surface had
acceptable bond strength. Bond failure analysis (adhesive remnant index) mainly showed adhesive bond
failures. An increased frequency of enamel fractures at debond was noted, with the control group (1) and the
MIP groups (3 and 5) having 22.5%, 12.5%, and 15%, respectively. The Assure groups had no enamel
fractures. (Am J Orthod Dentofacial Orthop 2002;122:267-73)

resins to etched enamel.11,12 Previous literature in

T
he development of the acid etch technique by
Buonocore1 in 1955 led to the direct bonding of
orthodontic brackets with composite resin. This
development resulted in improvements in orthodontic
treatment such as greater comfort for the patient,
elimination of pretreatment separation, decreased gin-
gival irritation, easier oral hygiene, improved esthetics,
and reduced chairside time.2-5 An area for clinical
improvement is the tolerance to moisture contamina-
tion during bonding to reduce the incidence of bond
failures.5
A reduction in bond strength of resins to etched
enamel after moisture and saliva contamination has
been reported by several researchers.6-10 Bonding
agents that contain hydrophilic monomers can counter-
act the negative effect of saliva on the bond strength of
From the Division of Graduate Orthodontics, University of Western Ontario,
London, Ontario, Canada.
a
Senior resident.
b
Associate professor, director of Graduate Clinic.
Reprint requests to: Timothy F. Foley, DDS, MCID, Director of Graduate Clinic,
Division of Graduate Orthodontics, University of Western Ontario, Dental Sci-
ences Bldg, London, Ontario, Canada N6A 5C1; e-mail, tfoley@uwo.ca.
Submitted, June 2001; revised and accepted, February 2002.
Copyright © 2002 by the American Association of Orthodontists.
0889-5406/2002/$35.00 ⫹ 0 8/1/126594
doi:10.1067/mod.2002.126594
restorative dentistry shows that bonding in a wet
environment is possible.5,7,11-14 The advent of resin-
modified glass ionomer adhesives (eg, Fuji Ortho LC,
GC America, Alsip, Ill) has demonstrated that ortho-
dontic bonding in a wet environment can be achieved,
and, indeed, such wet-field bonding is a criterion of the
resin-modified glass ionomer adhesive.5
In 1972, Wilson and Kent15 formulated “a new
translucent cement for dentistry,” glass ionomer cement
(GIC), which is a hybrid of silicate and polycarboxylate
cements and can bond physiochemically to both enamel
and dentin.16 Research dealing with hydrophilic GICs
demonstrated the advantage of releasing fluoride; how-
ever, these cements have generally shown poor bond
strengths compared with composite resins.9,17-20 In an
attempt to retain the positive attributes of GICs and
provide adequate bond strength, combinations of GICs
and composites have been developed. These hybrids
retain the favorable fluoride release and have improved
bond strengths. Resin-modified glass ionomer cements
(RMGICs) are GIC and composite combinations con-
sisting of 2 components that autoset by an acid-base
reaction of GICs and produce a diffusion-based adhe-
sion between the cement and the tooth surface.21
267
268 Schaneveldt and Foley
Polyacid-modified composite resins consist of similar
combinations but will not autoset by the acid-base
reaction of GICs. They behave more like resins.22
These cements have the unique ability to bond physio-
chemically to enamel.16 Widely varying bond strengths
for RMGICs have been reported, ranging from 5.39 to
18.9 MPa.23-27 Fricker28 reported a 5% bracket bond
failure rate for a RMGIC compared with an 8.3% bond
failure rate for a composite resin. Bond strengths for
polyacid-modified composite resins have been reported
in the range of 7.3 to 11.97 Mpa.20,27-29
One disadvantage of direct bonding has been mois-
ture control.30,31 A dry field is paramount for successful
bonding. In response to the competitive advantages of
RMGIC’s abilities in moist environments, manufactur-
ers have developed moisture-insensitive primers (MIP,
3M Unitek, Monrovia, Calif) and hydrophilic resin
systems (Assure, Reliance Orthodontic Products,
Itasca, Ill). A distinct advantage of hydrophilic adhe-
sives is in the treatment of impacted canines.30,31
Conventional composites that contain hydrophobic
functional monomers, which have little affinity to
enamel, work less well in cases of high impacted
canines when moisture control is impossible.31
Moisture-insensitive primers and hydrophilic resin
systems that have been recently introduced claim to
provide comparable bond strengths in a wet environ-
ment.5,11,13,14 Contamination can occur at 2 critical
times: after the tooth surface has been etched and after
the primer has been applied. Bonding could be com-
promised at both of these times.
There has been limited research concerning resin
adhesive bond strengths under saliva-contaminated
conditions.6,8,11,13,14 In response to the RMGICs, man-
ufacturers have developed moisture-insensitive primers
and resins to maintain an adequate level of bond
strength.6,8,11,13,14 Crane et al11 reported that moisture
contamination did not decrease the shear bond strength
of Fuji Ortho LC or Transbond XT (3M Unitek) with
MIP when bonded to etched enamel. However, Little-
wood et al32 found significantly lower bond strengths
with a new hydrophilic primer in a dry environment.
Hara et al33 reported clinically acceptable bond
strengths (15-24 MPa) under dry conditions for 4
hydrophilic adhesive systems (Scotchbond Multi-pur-
pose Plus, Stae, Single Bond, and Etch and Prime);
however, the bond strength of Etch and Prime was
significantly lower than that of the others. Rix et al34
and Grandhi et al35 also showed that moisture-insensi-
tive primers with their respective adhesives are effec-
tive in both wet and dry fields. Grandhi et al,35 using
bovine teeth, found that MIP was effective only in a
moist environment with a light-cured adhesive.
American Journal of Orthodontics and Dentofacial Orthopedics
September 2002
Recent studies6,8,11,13,14,32-35 using moisture-insen-
sitive primers vary widely with regard to sample size,
the use of human or bovine teeth, curing time, storage
before debonding, and thermocycling. As Fox et al36
pointed out, “If valid conclusions are to be drawn from
in vitro bond strength testing, at least 20 and preferably
30 specimens should be used per test.” Furthermore,
Buonocore37 advised thermal cycling of the specimens
to assess the durability of the bond. Otherwise, he
warned that “such results may not be indicative of the
effect on bond strength of long-term immersions under
oral moisture conditions.” The purpose of this study
was to investigate the effectiveness of moisture-insen-
sitive primers by comparing their shear-peel bond
strengths and adhesive-failure locations after contami-
nation with saliva.
MATERIAL AND METHODS
Two hundred forty extracted human premolars were
collected and stored in distilled water with thymol
crystals added to inhibit bacterial growth. Less than 6
months had elapsed between their extraction and the
bonding experiment. Teeth with restorations, enamel
defects, or abnormal cracking were excluded. The teeth
were numbered from 1 to 240 with a permanent marker
and randomly divided into 6 equal groups. Stainless
steel premolar brackets (.018-in MBT series without
hook, 3M Unitek) were bonded to the teeth with
different materials or procedures for each group. The
specimens were divided according to the method of
moisture contamination and primer-adhesive applica-
tion (Fig). The primers and adhesives were light cured
with a curing light (XL3000, 3M Unitek), which was
calibrated before use and then every 15 minutes to
ensure consistency.
Group 1, control (Transbond XT). The buccal sur-
face of each tooth was polished with a fluoride-free
pumice slurry, rinsed, and dried. The buccal surface
was then etched with 37% phosphoric acid for 30
seconds, rinsed for 15 seconds, and dried. A frosted
appearance indicated a successful etch. Transbond
primer was applied to the enamel surface in a thin film
and light cured for 10 seconds. Transbond XT adhesive
resin was applied to the bracket base; the bracket was
positioned on the buccal surface of the tooth and
pressed firmly into place to expel the excess adhesive.
The excess adhesive was removed and a light-cure unit
was used to cure the adhesive for 20 seconds on the
incisal edge and 20 seconds on the gingival edge of the
bracket.
American Journal of Orthodontics and Dentofacial Orthopedics
Volume 122, Number 3
Fig. 1 Diagrammatic representation of study specimen group.
Contamination before application of primer
Group 2 (Assure primer with Assure resin). Pum-
ice, etch, rinse, and dry procedures were done similarly
to the control procedure. As in a similar study,34 a thin
coat of natural saliva from the principal investigator
(S.S.) was applied with a brush to the etched and dried
enamel surface just before the application of Assure
primer. Assure primer was applied in 2 coats to the
prepared buccal surfaces, left for 10 seconds, lightly
dried, and light cured for 10 seconds. Assure adhesive
was then applied to the bracket base, and the bracket
was placed and bonded according to the control proto-
col.
Group 3 (MIP with Transbond XT). Pumice, etch,
rinse, and dry procedures were done similarly to the
control procedure. A thin coat of natural saliva was
applied to the etched and dried enamel surface just
before the application of MIP. MIP was applied to the
enamel surface in a thin film and light cured for 10
seconds. Transbond XT was bonded according to the
control protocol.
Contamination after application of primer
Group 4 (Assure primer with Assure resin). Pum-
ice, etch, rinse, and dry procedures were done similarly
to the control procedure. Assure primer was applied in
2 coats to the prepared buccal surfaces, left for 10
seconds, lightly dried, and light cured for 10 seconds. A
thin coat of natural saliva was applied to the primed
enamel surface. An additional layer of primer was
placed over this wet surface. Assure adhesive was then
applied to the bracket base and placed and bonded
according to the control protocol.
Group 5 (MIP with Transbond XT). Pumice, etch,
rinse, and dry procedures were done similarly to the
control procedure. MIP was applied to the enamel
surface in a thin film and light cured for 10 seconds. A
thin coat of natural saliva was applied over the primer.
Another thin coat of MIP was applied over this wet
surface and light cured for 10 seconds. Transbond XT
resin was then applied to the base of the bracket and
bonded aaccording to the control protocol.
Schaneveldt and Foley 269
Contamination after primer followed by bonding of
resin
Group 6 (Assure primer with Assure resin). Pum-
ice, etch, rinse, and dry procedures were done similarly
to the control procedure. Assure primer was applied in
2 coats to the prepared buccal surfaces, left for 10
seconds, lightly dried, and light cured for 10 seconds. A
thin coat of natural saliva was applied to the primed
enamel surface. Assure adhesive was then applied to
the bracket base, placed, and bonded according to the
control protocol.
The bracketed teeth were stored in deionized water
in sealed containers and placed in an incubator at 37° C
for 30 days. After that, the teeth were thermocycled in
2 thermally controlled streams of water maintained at
10°C and 55°C for 24 hours (30-second intervals
between cycles). An 0.018 ⫻ 0.025-in stainless steel
wire was ligated into each bracket slot. Each tooth was
mounted in an acrylic block. The brackets were
debonded with a shear-peel load parallel to the bracket
base with a testing machine (Instron, Canton, Mass)
with a 50-kg load cell and a crosshead speed of 2.0
mm/min. The load applied at failure was recorded in
kilograms and the bond strength in megapascals {(load
in kg/bracket base area [10.61mm2]) ⫻ 9.81 (the
gravitational acceleration constant)}. With a 16⫻ mag-
nification, the debonded enamel surfaces were exam-
ined to assess the residual adhesive remaining on the
teeth by using the adhesive remnant index (ARI) as
described by Artun and Bergland38 and modified by
Meehan et al27 to include a score of enamel fracture
(EF).
A 1-way analysis of variance and Tukey multiple
comparison tests were used to determine statistically
significant differences among the mean shear-peel bond
strengths of the 6 groups. The percentage and fre-
quency of ARI fracture types recorded were analyzed
by a chi-square test.
RESULTS
The mean shear-peel bond strengths (megapascals)
and SD of the bond strengths for the 6 groups are
270 Schaneveldt and Foley American Journal of Orthodontics and Dentofacial Orthopedics
September 2002

Table I. Shear-peel bond strengths (MPa)

Group Mean SD Minimum Maximum Group

Transbond XT (group 1) 14.82 2.62 10.6 19.4 A

Assure wet preprimer (group 2) 9.00 2.10 5.5 14.8 C
MIP wet preprimer (group 3) 12.23 2.53 8.3 18.0 B
Assure wet intraprimer (group 4) 11.41 3.28 5.1 20.3 B
MIP wet intraprimer (group 5) 14.02 2.94 9.7 19.0 A
Assure wet postprimer (group 6) 9.28 1.93 6.9 13.9 C

Similar letters connect statistically equivalent groups.

Table II. Frequency of adhesive remnant index scores (%)

Group ARI ⫽ 0 ARI ⫽ 1 ARI ⫽ 2 ARI ⫽ 3 EF

Transbond XT (group 1) 2.5 15.0 42.5 17.5 22.5

Assure wet preprimer (group 2) 0.0 47.5 40.0 12.5 0.0
MIP wet preprimer (group 3) 0.0 47.5 17.5 22.5 12.5
Assure wet intraprimer (group 4) 2.5 17.5 50.0 30.0 0.0
MIP wet intraprimer (group 5) 0.0 20.0 25.0 40.0 15.0
Assure wet postprimer (group 6) 0.0 15.0 72.5 12.5 0.0

chi-square ⫽ 31.41 P ⬍ .001.

0, no adhesive on tooth; 1, ⬍50% adhesive on tooth; 2, ⬎50% adhesive on tooth; 3, all adhesive on tooth; EF, enamel fracture; ARI, adhesive
remnant index.

shown in Table I. All adhesives had clinically accept-
able bond strengths. The mean shear-peel bond
strengths of the control adhesive, group 1 (14.82 MPa),
and MIP group 5 (14.02 MPa), were significantly
greater than those of the 4 other groups (P ⬍ .001).
MIP group 3 had a mean bond strength (12.23 MPa)
that was significantly greater than that for Assure
groups 2 and 6 (9.00 and 9.28 MPa, respectively) but
was not significantly different from Assure group 4,
with contamination between 2 layers of the moisture-
insensitive primer (11.41 MPa). Both Assure group 4
and MIP group 5 showed significantly greater bond
strengths (14.02 and 11.41 MPa, respectively) than did
groups 2 and 3 (9.00 and 12.23 MPa, respectively).
The ARI scores were analyzed by using a chi-
square test (Table II); comparing the ARI scores
indicated significant differences among the various
adhesives. Transbond XT group 1 and MIP groups 3
and 5 had more EF than all the Assure groups. Both
Assure and MIP groups 2 and 3 had a greater frequency
of an ARI score of 1 (⬍50% of the adhesive remaining
on the tooth) than did the other groups. Both Assure
and MIP groups 4 and 5 had a greater frequency of an
ARI score of 3 (all adhesive remaining on the tooth)
than did the other groups.
DISCUSSION
The principles of modern adhesives are the
result of decades of research in restorative den-
tistry.5,12,15,18,21,22,28,29,32,37,39-44 The changes in the
different generations of bonding systems have pro-
gressed from etching enamel to etching-conditioning
dentin, smear layer treatment, and altered handling
properties of adhesives.45 The introduction of moisture-
insensitive primers to orthodontics stems from the
advances in restorative materials.45-48 The generational
improvements in bonding primers for restorative den-
tistry, listed by characteristic, surface treatment, and
properties, respectively, are as follows: first generation,
N-phenylglycine and glycidl methacrylate (NPG-
GMA), etched enamel, and dry bonding; second gen-
eration, bis-GMA/HEMA, etched enamel, and dry
bonding; third generation, 4-META/BPDM, etched
enamel surface, and dry bonding; fourth generation,
hydrophilic primer, etched enamel/dentin, and wet
bonding; and fifth generation, 1-bottle systems, etched
enamel/dentin, and wet bonding.
Wet bonding or bonding in a moist environment
was achieved in the fourth generation and applies to
orthodontic bonding. Fifth-generation bonding systems
were developed to minimize the steps and increase the
reliability of bonding. Two different types of materials
were introduced, 1-bottle systems and self-etching
primer bonding systems. One-bottle systems combined
the primer and adhesive in 1 solution that is applied
after the total etching technique.41 The self-etching
primer bonding system is an aqueous solution of
phenyl-P in HEMA and has the advantages of reduced
American Journal of Orthodontics and Dentofacial Orthopedics
Volume 122, Number 3
working time by eliminating the rinsing step of the
acidic gel and less risk of collagen collapse.42 Fifth-
generation systems have simplified the bonding proce-
dure by reducing the steps, but this has been achieved
at the expense of lower bond strengths.47 Chung et al,48
using fourth-generation primers or adhesion boosters,
showed increased bond strength as compared with no
boosters, whereas the current study and Littlewood et
al32 showed lower bond strength with the fifth-genera-
tion MIP primer compared with a conventional primer.
Grandhi et al,35 using bovine teeth, found similar bond
strengths for both the conventional Transbond primer
and the MIP primers in dry-etched conditions.
Although occlusal loads show enormous individual
variability, the bond strengths of all the adhesives
tested were greater than the 5 to 8 MPa that is
considered adequate for attaching orthodontic brackets
to enamel49 under tensile load; however, the clinical
acceptable shear bond strength for orthodontic brackets
to enamel is still unknown. The methodology for
testing bond strength in this study was similar to that
reported by Meehan et al27 and Lalani et al,50 who
found mean shear debond loads of 11.23 and 11.31
MPa, respectively, that were necessary to dislodge
light-cured metal brackets bonded to buccal surfaces
with Transbond XT. The mean shear debond loads for
the 6 groups in this study ranged from 9.00 to 14.82
MPa, indicating that acceptable bond strengths for
orthodontic treatment purposes were achieved with all
the adhesives. The bond strength of group 1 (Transbond
XT) at 14.82 MPa was significantly greater than the
bond strengths of the other adhesives in this study,
except MIP group 5 (14.02 MPa), and was similar to
that found in previous studies.5,23,25,27,50 The bond-
strength values of MIP primer and Transbond XT
determined by Grandhi et al35 were lower than in the
current study, which should be expected when using
bovine enamel. Oesterle et al51 found bond strengths to
bovine enamel to be 21% to 44% weaker than to human
enamel. Rix et al34 found slightly stronger bond
strength values (10.99 MPa compared with 9.00 MPa
recorded in the current study) when Assure primer was
placed on a contaminated, etched surface. Littlewood et
al32 found that brackets bonded with a new hydrophilic
primer under dry conditions had significantly lower
bond strengths than those bonded with a conventional
primer (Transbond); this was similar to the findings of
this study. In contrast to Littlewood et al,32 bond
strengths found in the current study were clinically
acceptable. Assure and MIP groups 4 and 5 showed
mean shear-bond strengths of 11.41 and 14.02 MPa,
respectively, and were significantly greater than their
corresponding groups 2 and 3 (9.00 and 12.23 MPa,
Schaneveldt and Foley 271
respectively). These higher bond strengths might sug-
gest larger amounts of contaminated components, or-
ganic and inorganic substrates in saliva, remaining on
the etched surfaces and preventing complete penetra-
tion of the primer.8 Itoh et al9 reported that insoluble
saliva proteins and minerals compromise the setting of
the cements; it is possibly more significant that the high
viscosity of saliva that might occlude the microscopic
roughness produced by etching inhibits proper resinous
tag formation.
To standardize the direction of the debonding force,
we mounted each specimen in acrylic blocks; however,
Fox et al36 cautioned that a pure shear test might not be
ensured, and factors such as the curvature of the enamel
surface might influence the results. O’Brien et al52
determined that the ARI score depended on many
factors, including the bracket base design and the
adhesive type, and not simply on the bond strengths at
the interfaces. Furthermore, ARI values are subjective.
Nevertheless, the index was useful in determining the
percentage of bond-failure sites by ranking the amount
of resin remaining on the tooth after debond. The ARI
scores for this study displayed a higher frequency of EF
on debonding for Transbond XT and MIP groups 1, 3,
and 5. In this study, the frequency of EF for group 1
was 22.5% compared with similarly treated samples by
Lalani et al50 (16.2%) and Rix et al34 (57.5%). The
increased EF at debond might be related to the in-
creased enamel cracking as a result of extraction forces
before bonding and the in vitro test methods.34 In this
study, the frequency of EF increased with the materials
that had the greatest bond strengths: Transbond XT
group 1 (14.82 MPa) and MIP groups 3 and 5 (12.23
and 14.02 Mpa, respectively). Both Assure group 2
(9.00 MPa) and MIP group 3 (12.23 MPa) had a greater
frequency of an ARI score of 1 (⬍50% of the adhesive
remaining on the tooth), indicating more frequent
failures at the enamel/adhesive interface.
CONCLUSIONS
1. Both bonding systems provide adequate bond
strengths whether saliva contamination occurs be-
fore or after the application of the hydrophilic
primers; therefore, additional mechanical prepara-
tion and re-etching of the enamel surface after saliva
contamination might not be required.
2. Comparing saliva contamination after application of
primer, both MIP and Assure had significantly
greater shear-peel bond strengths than when con-
tamination occurred before the application of each
primer.
3. Transbond XT and MIP group 5 (contamination
between 2 layers of primer) showed significantly
272 Schaneveldt and Foley
greater shear-peel bond strengths compared with the
other groups.
4. The groups with saliva contamination before appli-
cation of the primer showed more frequent failures
at the enamel/adhesive interface, suggesting that
complete penetration of primer was prevented,
whereas the groups with saliva contamination after
the first application of primer showed more frequent
failures at the adhesive/bracket interface.
5. The greatest frequencies for EF on debonding oc-
curred in the groups with the highest bond strengths.
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