THE JOURNAL OF - Dentsply

THE JOURNAL OF 

ADHESIVE 

DENTISTRY 

VOLUME 9 • SUPPLEMENT 2 

2007

All inclusive 

bondi Etch Bond Easy Bond 

Fast Bond Slow Bond Mega Bond XP BOND 

NEW! 

Universal Total-Etch Adhesive 

* For indirect indications in combination with DENTSPLY Self Cure Activator. 

There are many adhesives available. Some bond a little better, others are 

easy to use and again others are more forgiving. The new total-etch adhesive 

XP BOND unites all these attributes in one single product. 

XP BOND stands out because it delivers superior bonding performance 

combined with easy handling and a high degree of technique tolerance. 

Moreover, it is truly universal for all kinds of direct and indirect indications.* 

Who needs the rest, when you can have it all inclusive

Guest Editorial 

Satellite Symposium on Dental Adhesives, 

Dublin, September 13th, 2006 

Dear ColIeagues, 

I clearly remember the moment: During a German conservative 

dentistry congress focusing on adhesive vs conventional 

techniques in 2004, one of my colleagues said: “I do 

not think that ‘adhesive dentistry’ really exists. Okay, there 

is even a journal named like that. I admit that there may be 

something like an adhesive technique in dentistry, but I don’t 

think this is really a discipline.” 

Now, two years later with the previously mentioned journal 

having received an impact factor of more than 2.2, the 

world can see how important this discipline has become in 

the dental literature. 

For decades, Dentsply has been one of the leading companies 

dealing with adhesion. This supplement is the scientific 

result of a satellite symposium held in Dublin on September 

13th, 2006, prior to the annual IADR/CED/PEF 

meeting just around the corner from famous Trinity College. 

Experts from all over the world (USA, Germany, Belgium, 

Spain, Italy) met to exchange experiences with established 

adhesive materials and the most recent Dentsply development, 

XP-Bond. We learned that Dentsply’s Sevriton actually 

was the first adhesive approach, dated years before 

Buonocore’s fundamental publication. We heard that fatigue 

measurement is one major tool in preclinical testing 

and that differences in performance during in vitro testing 

blur between etch-and-rinse and self-etching adhesives; it is 

becoming more important to look at the individual product. 

However, clinical trials are still the ultimate instrument to investigate 

dental biomaterials, such as bonded resin composites 

or ceramic inlays. 

It is an honor for me to welcome you to this supplement 

of the Journal of Adhesive Dentistry, 2007. Enjoy reading! 

Sincerely, 

Roland Frankenberger 

Vol 9, Supplement 2, 2007 223

Sarrett 

260 The Journal of Adhesive Dentistry


ADHESIVE 

DENTISTRY 

Contents Volume 9 • Supplement 2, 2007 

Editorial 

Reviews 

223 

227 

231 

241 

245 

249 

255 

261 

265 

269 

275 

279 

Satellite Symposium on Dental Adhesives, Dublin, September 13th, 2006 

Roland Frankenberger 

Dental Adhesives …. How it All Started and Later Evolved 

Karl-Johan M. Söderholm 

Effectiveness of All-in-one Adhesive Systems Tested by Thermocycling Following 

Short and Long-term Water Storage 

Uwe Blunck/Paul Zaslansky 

Clinical Bonding of a Single-step Self-etching Adhesive in Noncarious Cervical 

Lesions 

Jan WV van Dijken/Karin Sunnegårdh-Grönberg/Ebba Sörensson 

Shear Bond Strength and Physicochemical Interactions of XP BOND 

Mark A. Latta 

Microshear Fatigue Testing of Tooth/Adhesive Interfaces 

Marc Braem 

Microleakage of Class V Composite Restorations Placed with Etch-and-Rinse 

and Self-etching Adhesives Before and After Thermocycling 

Juan Ignacio Rosales-Leal 

Microleakage of XP BOND in Class II Cavities After Artificial Aging 

Jürgen Manhart/Cordula Trumm 

Six-month Clinical Evaluation of XP BOND in Noncarious Cervical Lesions 

Uwe Blunck/Katharina Knitter/Klaus-Roland Jahn 

Adhesive Luting Revisited: Influence of Adhesive, Temporary Cement, Cavity 

Cleaning, and Curing Mode on Internal Dentin Bond Strength 

Roland Frankenberger/Ulrich Lohbauer/Michael Taschner/Anselm Petschelt/ 

Sergej A. Nikolaenko 

XP BOND in Self-curing Mode used for Luting Porcelain Restorations. 

Part A: Microtensile Test 

Ornella Raffaelli/Maria Crysanti Cagidiaco/Cecilia Goracci/Marco Ferrari 

XP BOND in Self-curing mode used for Luting Porcelain Restorations. 

Part B: Placement and 6-month Report 

Marco Ferrari/Ornella Raffaelli/Maria Crysanti Cagidiaco/Simone Grandini 



ADHESIVE 

DENTISTRY 

Editors-in-Chief 

Prof. Dr. 

Jean-François Roulet 

Escher Str. 9 

FL 9494 Schaan, Liechtenstein 

Tel: ++423 232 1632 

Fax: ++423 239 4632 

Mobile phone +41 79 311 4673 

E-mail: jfroulet@aol.com 

Submit the manuscripts and 

illustrations preferably through: 

www. manuscriptmanager.com/jadd 

Or mail to: 

Quintessenz Verlags-GmbH, 

Juliane Richter 

The Journal of Adhesive Dentistry, 

Ifenpfad 2-4, D-12107 Berlin, Germany 

Editorial Board 

Antonson, S. (USA) 

Assmussen, E. (Denmark) 

Attal, J.-P. (France) 

Bayne, S. (USA) 

Blatz, M. (USA) 

Blunck, U. (Germany) 

Bouillaguet S. (Switzerland) 

Brabant, A. (Belgium) 

Burrow, M. (Australia) 

Burtscher, P. (Liechtenstein) 

Carvalho, R. (Brazil) 

Cognard, J. (Switzerland) 

Creugers, N. (Netherlands) 

Davidson, C.L. (Netherlands) 

Dejou, J. (France) 

Dietschi, D. (Switzerland) 

Eliades, G. (Greece) 

Erickson, R.L. (USA) 

Ferracane, J. (USA) 

Ferrari, M. (Italy) 

Finger, W. (Germany) 

Frankenberger, R. (Germany) 

Fuzzi, M. (Italy) 

Glantz, P.-O. (Sweden) 

Heintze, S. (Liechtenstein) 

Hickel, R. (Germany) 

Jacobsen, T. (Sweden) 

Jahn, K.-R. (Germany) 

Janda, R. (Germany) 

Kern, M. (Germany) 

Kreulen, C. (Netherlands) 

Kugel, G. (USA) 

Kulmer, S. (Austria) 

Kunzelmann, K.-H. (Germany) 

Lambrechts, P. (Belgium) 

Liebenberg, W. H. (Canada) 

Lynch E. (Irland) 

Macorra de la, J.C. (Spain) 

Matsumura, H. (Japan) 

Mehl, A. (Germany) 

Momoi, Y. (Japan) 

Munksgaard, Ch. (Denmark) 

Nakabayashi, N. (Japan) 

Navarro, F. (Brazil) 

Nikaido, T. (Japan) 

Noack, M.J. (Germany) 

Özcan, M. (Netherlands) 

Pashley, D. H. (USA) 

Paul, S. J. (Switzerland) 

Perdigao, J. (USA) 

Peutzfeld, A. (Denmark) 

Powers, J. M. (USA) 

Prati, C. (Italy) 

Qvist, V. (Denmark) 

Ruse, D. (Canada) 

Salz, U. (Liechtenstein) 

Samama, Y. (France) 

Sano, H. (Japan) 

Schultz, J. (France) 

Senda A. (Japan) 

Simonsen, R.J. (USA) 

Söderholm, K.-J. (USA) 

Spreafico, R. (Italy) 

Städtler, P. (Austria) 

Suzuki, S. (USA) 

Tay, F. (China) 

Thompson, V. P. (USA) 

Toreskog, S. (Sweden) 

Triolo, P. T. (USA) 

Tyas, M. J. (Australia) 

Vallittu, P. (Finland) 

Van Noort, R. (United Kingdom) 

Vargas, M. (USA) 

Watson, T. (United Kingdom) 

Wilson, N. H. F. (United Kingdom) 

Statistical Consultant 

Fischer T. H. (Germany) 

Hopfenmüller, W. (Germany) 

ISSN 1461-5185 

Prof. Bart Van Meerbeek 

Catholic University of Leuven 

Department of Conservative Dentistry 

Kapucijnenvoer 7 

B-3000 Leuven, Belgium 

Tel: ++32 16 337587 

Fax: ++32 16 332752 

E-mail: Bart.Vanmeerbeek@ 

med.kuleuven.ac.be 

The Journal of Adhesive Dentistry publishes scientifically sound articles of interest 

to practitioners and researchers in the field of adhesion to hard and soft dental 

tissues. Included are clinical and basic science research reports based on original 

research in adhesive dentistry and related subjects, review articles on topics 

related to adhesive dentistry, as well as invited focus articles with commentaries. 

The Journal of Adhesive Dentistry is Indexed in Science Citation Index Expanded, 

ISI Alerting Services, and Current Contents/Clinical Medicine. 

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Dental Adhesives …. How it All Started and Later Evolved 

Karl-Johan M. Söderholm a 

Abstract: This article describes how dental adhesives evolved from the cements developed by the Mayan Indians into 

today’s modern dental adhesives. Particular attention is paid to Oskar Hagger, a chemist who worked for DeTrey/Amalgamated 

Dental Company, and already in 1949 developed an adhesive product called Sevriton Cavity Seal. That adhesive 

was acidic and interacted with the tooth surface on a molecular level. His ground-breaking concept makes him the 

true “Father of Modern Dental Adhesives.” Hagger’s concept was soon adopted by other investigators, and different generations 

of dental adhesives evolved thereafter. Today, after many years of accepting that the key to the success of dental 

adhesives is the micromechanical retention resulting from acid etching of dentin and enamel, we still return to Dr. 

Hagger’s original concept that bonding can be achieved via molecular interactions between adhesives and tooth surfaces. 

That concept is obvious in the development of newer generations of dentin adhesives. These adhesives, like Sevriton 

Cavity Seal, rely on acidic monomers capable of etching and interacting on a molecular level with tooth surfaces in 

order to form physical/chemical bonds between the restoration and the tooth. Whether Hagger’s concept will become 

the norm in the future is still an open question, but one thing is certain: Hagger’s idea is still very much alive. 

Keywords: review, generations, clinical evaluations. 

J Adhes Dent 2007; 9: 227-230. Submitted for publication: 15.12.06; accepted for publication: 4.1.07. 

a Professor, Department of Dental Biomaterials, College of Dentistry, University 

of Florida, Gainesville, FL, USA. 

Paper presented at Satellite Symposium on Dental Adhesives, Dublin, 

September 13th, 2006. 

Reprint requests: Prof. Karl-Johan M. Söderholm, Department of Dental Biomaterials, 

College of Dentistry, College of Dentistry, 1600 SW Archer Road, 

Gainesville, FL 32610-0446, USA. Tel: +1-352-392-0575, Fax: +1-352-392-7808. 

e-mail: ksoderholm@dental.ufl.edu 

In 1955, Buonocore published a paper entitled “A simple 

method of increasing the adhesion of acrylic filling materials 

to enamel surfaces”. 15 That paper is often regarded as 

the foundation of adhesive dentistry, and today that paper 

is the 17th most cited paper published in the Journal of Dental 

Research since March of 1919. 

Buonocore’s paper 15 clearly outlined different approaches 

to obtain bonding between filling materials and tooth 

structure. These approaches included: (a) the development 

of new materials which have adhesive properties, (b) modification 

of present materials to make them adhesive, (c) the 

use of coatings as adhesive interface materials between filling 

and tooth, and (d) the alteration of the tooth surface by 

chemical treatment to produce a new surface to which present 

materials might adhere. 

In the 1955 paper, Buonocore focused on the (d) alternative 

by targeting enamel bonding. He believed that treatment 

of intact enamel surfaces would have only limited application 

to the broader problems of restorative dentistry. He 

focused on enamel etching because he had found that phosphoric 

acid or preparations containing phosphoric acid had 

been used to treat metal surfaces in order to obtain better 

adhesion of paint and different resin coatings. 

Obviously, Buonocore used knowledge from other disciplines 

and transferred that knowledge to dentistry. What 

Buonocore did not seem to consider was that the Mayan Indians 

in pre-Columbian times had used acidic cements to attach 

their semi-precious stone inlays. 20 He also forgot to 

consider that several acidic cements had been used by dentists 

more than a hundred years before he invented acid 

etching, 27 and that a common zinc phosphate cement was 

a mixture of zinc oxide and phosphoric acid. 37 It was well 

known that during setting, these cements remained 

acidic. 40 What Buonocore forgot was that these cements 

were also able to etch tooth surfaces and increase the surface 

roughness. During setting, formed setting compounds 

grew into the surface roughnesses created by the acidic cement. 

Because of mechanical interlocking between tooth, 

cement, and crown, retention of the cemented restoration 

could be achieved. Considering that the Maya were the first 

to use acidic cements, a legitimate question is whether 

Buonocore really was the one who invented acid etching or 

if that honor shouldn’t go to the Maya. Buonocore’s true contribution 

was that he opened our eyes to make us aware of 


Söderholm 

Fig 1 Sevriton and Severiton Cavity seal were products developed 

by the DeTrey/Amalgamated Dental Company. Sevriton Cavity 

Seal was the first product claimed to be able to bond to tooth 

tissues. 29 This product was developed by the Swiss chemist, 

Oskar Hagger. 

the fact that microscopic porosities enhanced the retention 

of dental materials. What he did not communicate clearly, 

though, was that by replacing a brittle cement layer with a 

ductile material, the bonding ability could be substantially 

enhanced. The latter fact was probably the reason why the 

acid etching technique resulted in a major breakthrough in 

dentistry when compared to previous approaches to bonding 

to teeth. 

However, when it comes to a ductile interface, Buonocore 

was not the first to use a ductile resin layer at the tooth surface 

in order to enhance retention. The first one who came 

up with that idea was a Swiss chemist, Oskar Hagger. Hagger 

worked for DeTrey/Amalgamated Dental Company, and 

had already in 1949 developed an adhesive product called 

Sevriton Cavity Seal 33 (Fig 1). This product consisted of glycerolphosphoric 

acid dimethacrylate and was intended for 

use as an adhesive for the chemically cured resin Sevriton. 

Sevriton Cavity Seal was indeed a revolutionary product, because 

it was the first product that claimed to be able to 

chemically bond to tooth structure. In an article published by 

Kramer and McLean in 1952, 29 these two investigators 

claimed that the glycerolphosphoric acid dimethacrylate of 

the Sevriton Cavity Seal increased the adhesion to dentin by 

penetrating the surface. Today we call the resin-penetrated 

zone the hybrid zone. This is also remarkable, because we 

often assume that hybridization is a more recent discovery 

than it obviously is. 

The year after Buonocore published his classic paper, he 

also published a paper with Brudevold and Wileman, 13 in 

which they evaluated Sevriton Cavity Seal and Sevriton. In 

that paper they claimed that the glycerolphosphoric acid 

dimethacrylate did not bond as well to enamel as a self-curing 

resin placed in intimate contact with a phosphoricacid–etched 

enamel surface did. However, when placed in 

contact with dentin, the glycerolphosphoric acid dimethacrylate 

provided some dentin bond enhancement. 

Considering Hagger’s fundamental work, there is no 

doubt that modern dental adhesive technology had its root 

in the late 1940s, when Hagger initiated the use of acidic 

monomers to achieve bonding to both enamel and dentin. 

What Buonocore really showed was that it was easier to 

achieve bonding to enamel than to dentin, something we all 

agree upon today. 

Even though Buonocore had proved that enamel bonding 

worked in 1955, 15 it would take until the late 1970s before 

enamel bonding became generally accepted. The turning 

point occurred when 3M sponsored the International Symposium 

on Enamel Etching in December of 1974. 38 During 

that symposium, researchers and clinicians with experience 

of enamel bonding presented their findings, and 3M published 

and distributed that information to academic institutions 

and opinion leaders. 

The idea to develop a resin system capable of bonding to 

dentin did not die with Hagger. Instead, Bowen, after his invention 

of modern composites, focused on dentin adhesives 

during the 1960s. During that decade, he formed work 

groups that outlined strategies for developing new dental adhesives. 

7-11 Guiding principles during these discussions 

were: (a) dentin is a vital tissue and should not be exposed 

to strong acids, (b) the presence of water should be minimized, 

because water would shield bond sites of adhesive 

molecules, (c) the adhesive molecules should be at least bifunctional 

so one end could bond to tooth surface and the 

other to the resin of the composite. 

As a result of Bowen’s research, NPG-GMA (N-phenylglycine 

and glycidyl methacrylate) was introduced in 1965 as 

a potential dentin adhesive. The shear bond strength of this 

first generation adhesive was 1 to 3 MPa, and it soon became 

obvious that these products did not work clinically. 

During the late 1970s, new dentin adhesives were developed. 

Most of these products contained of bis-GMA/HEMA 

resins mixed with halophosphorous esters. The bonding 

mechanism of these adhesives was believed to be due to 

ionic bond formation between halophosphorous groups and 

calcium ions of the tooth surface. Even though these second 

generation products were significant improvements compared 

to the first generation products, they still did not result 

in clinical success. 

A major breakthrough occurred in 1979, when Fusayama 

and his coworkers presented their findings, claiming they 

could bond to acid-etched dentin without any significant 

problems with pulp reactions. 22 The paper was met with ample 

skepticism by authorities in pulp biology who argued 

that the acidity would cause pulp inflammations and even 

pulp necrosis. Fusayama, on the other hand, argued that his 

findings were just supporting Brännström and Nyborg’s 

claim that bacteria rather than acid was the key concern 

when it came to causing pulp damage. 12 

Another important paper from Japan came in 1982, 

when Nakabayashi and coworkers published their paper 

“The promotion of adhesion by the infiltration of monomers 

into tooth substrates”. This paper presented the hybrid-layer 

formation theory. 35 

The findings from Fusayama’s and Nakabayashi’s groups 


Söderholm 

resulted in a new generation of adhesives, the so-called 3rd 

generation adhesives. Manufacturers of adhesives were still 

somewhat reluctant to suggest an aggressive acid etching of 

the dentin. Instead, they tried to remove or modify the smear 

layer with a conditioner (often a weaker acidic solution) that 

was rinsed away before a hydrophilic primer was placed. 

These primers often consisted of 4-META and BPDM, and after 

primer application, an unfilled resin was placed. Other 

primers contained PENTA, HEMA and ethanol. One product 

used EDTA instead of acid to remove the smear layer and expose 

the collagen, and treated the exposed collagen fibers 

first with an aldehyde and then HEMA. 34 With that treatment, 

it was believed that the aldehyde would chemically 

bond to the collagen fiber and that the HEMA would then 

bond to the attached aldehyde molecules via a condensation 

reaction. The methacrylate groups of the HEMA molecule 

would then react with the composite. 

Interesting to mention is that Bowen and Cobb published 

a paper in 1983 entitled “A method for bonding to dentin 

and enamel”, 6 in which they claimed they could achieve an 

in vitro tensile bond strength corresponding to one ton per 

square inch. Translated into metric units, that would be 15.5 

MPa. The bonding procedure was rather complex, but in that 

article, Bowen regarded this approach as a major breakthrough 

despite its complexity. 

Even though the 3rd generation adhesives were improvements, 

they did not result in long-term success. In 

1985, Hansen and Asmussen correlated gap sizes around 

standardized cavities with the shear bond strength and 

found that gap-free restorations would be possible at shear 

bond strength values of around 23 MPa. 25 The best adhesives 

then had shear strength values of 18 MPa. 

Toward the end of the 1980s, some interesting research 

was published. The first paper came in 1985, when Bowen 

presented an abstract at an IADR meeting that contained information 

on the NTG-GMA he had been so enthusiastic 

about in his and Cobb’s 1983 publication. 5 In the 1985 presentation, 

he revealed that the adhesive he had used in 

1983 contained an impurity. That impurity was nitric acid, 

and after purifying, the bond strength declined substantially. 

What he inadvertantly showed was how important it was 

to etch the dentin surface. 

Another important finding came in 1989, when Chigira et 

al treated an EDTA-conditioned dentin surface with aldehyde 

plus HEMA or HEMA only and found no difference in 

bond strength. 17 What they showed with that study was that 

collagen exposure and resin infiltration was the key behind 

dentin bonding, thereby supporting Nakabayashi’s hybridization 

theory. 

Some of the most important information came in 1994, 

when Van Herle’s group at the Catholic University of Leuven 

showed in a clinical study that the success rate of Scotchbond 

2, a third generation dentin adhesive, exceeded 95% after 3 

years. 43 Because of poor storage stability, Scotchbond 2 disappeared 

from the market almost immediately after it had 

been accepted and was replaced by Scotchbond MP, a 4th 

generation adhesive. At that time, it had started to become 

clear that by using more aggressive dentin treatments, the 

bond strength improved and exceeded the levels predicted by 

Hanssen and Asmusen for gap-free restorations. 25 

Even though Fusayama and later on Nakabayashi had 

done extensive research on dentin etching and dentin bonding 

during the 1980s, it was during the early 1990s that 

dentin etching and dentin bonding first became widely accepted. 

The acceptance coincided with a symposium sponsored 

by 3M and later on published in Operative Dentistry. 4 

Another important discovery was when Kanka 28 and Gwinnett 

24 in two independent papers showed that bonding to 

dentin could be enhanced by using so-called moist bonding. 

Knowledge transfer is rarely an easy task, and when it 

came to introducing the 4th generation adhesives to the 

dental profession, it was soon clear that dentists did not really 

know how to do dentin bonding. Sometimes different 

components were used in the wrong order, and when it came 

to moist dentin, the definition differed quite widely. Because 

of these factors, there was a need for products that were 

easier to use, a demand to which the manufacturers soon 

responded. 

In an attempt to simplify dentin bonding, the primer and 

adhesive resin were combined. Unfortunately, the general 

perception among clinicians was often that by using a 5th 

rather than a 4th generation adhesive, the time needed for 

the bonding procedure could be decreased. In reality, 

though, such a belief was incorrect, because these systems 

required more time for the primer to diffuse into the collagen 

structure. Clinical studies that came out comparing the 4th 

and the 5th generation adhesives often suggested that the 

4th generation adhesives performed somewhat better than 

the 5th generation adhesives. 1,14,31,42 Whether that difference 

was due to 5th generation adhesives curing too quickly 

has not been proven. However, in vitro results of different 

generation adhesives can be similar, independent of generation. 

19 

Simultaneously with the introduction of the 5th generation 

adhesives, new adhesives consisting of an acidic primer 

and an adhesive were also introduced. These systems often 

came from Japanese manufacturers of dental adhesives, 

and did not include the etching gel. Because of the generation 

terminology, these systems are referred to as the 6th 

generation of adhesives. 

In 1998, a new adhesive named Prompt-L-Pop was introduced, 

consisting of a delivery system that mixed the primer 

and the adhesive before it was applied. The popularity of this 

system grew quickly and it soon became quite clear that the 

market wanted a system that was self-etching and available 

in one single container. During the past few years, the trend 

has been to move the adhesive one step further by combining 

the acidic primer with the adhesive resin in an attempt 

to develop an all-in-one system, often marketed as 7th generation 

adhesives. 

The interest in the 7th generation products has been 

quite significant, despite the fact that these systems often 

perform less satisfactorily than many of the previous generation 

adhesives. 39 However, it is important to emphasize 

that all products, including the 7th generation adhesives, 

have learning curves. The knowledge generated during 

these trial periods is used to develop and improve products 

that do not perform as well as originally believed. Unfortunately, 

these development periods can be quite frustrating 

for the clinicians when faced with patients who have re- 


Söderholm 

ceived a restoration that later fails. Today, most research indicates 

that the 4th generation adhesives still serve as the 

gold standard, but because of the interest dentists show in 

the 7th generation adhesives, it seems clear that dentists 

want simple-to-use adhesives. Because of that wish, they are 

willing to explore adhesives that are easier to use, despite 

the risk that they may have more failures with such products. 

Thanks to what has been learned during that cycle of the 

evolution process, these easier-to-use products have 

evolved during the past few years, and today it seems that 

the clinical success rate of 7th generation adhesives is approaching 

that of the 4th generation adhesives. 2,3,16,18,21,23, 

26,30,32,36,41,44 

By looking back at adhesives, we must admit that 

progress has been made since Hagger’s idea that resins 

could be bonded to tooth surfaces. Nevertheless, we should 

also remember that in 1949, when Hagger came up with his 

revolutionary idea to use glycerolphosphoric acid dimethacrylate 

in Sevriton Cavity Seal, he had in fact invented a selfetching 

adhesive. Based on the definitions, we can classify 

Sevriton Cavity Seal as a 7th generation adhesive. Perhaps 

improvements of dental materials don’t occur as fast as 

many of us believe. 

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Am J Dent 1996;9:77-79. 

2. Aw TC, Lepe X, Johnson GH, Mancl L. One-year clinical evaluation of an 

ethanol-based and a solvent-free dentin adhesive. Am J Dent 2004;17:451- 

456. 

3. Aw TC, Lepe X, Johnson GH, Mancl LA. A three-year clinical evaluation of twobottle 

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2004;29:376-385. 


Effectiveness of All-in-one Adhesive Systems Tested by 

Thermocycling Following Short and Long-term Water 

Storage 

Uwe Blunck a /Paul Zaslansky b 

Purpose: To evaluate and compare the marginal integrity of in vitro Class V restorations made with all-in-one adhesive 

systems by thermocycling after different periods of water storage, to provide an analysis of static and quasi-dynamic 

deterioration in water. 

Materials and Methods: Standardized Class V cavities (17 groups, 8 specimens each) were prepared in extracted 

human caries-free anterior teeth. The cavities were filled using 14 all-in-one adhesive systems/composite resin combinations 

in addition to the multi-bottle adhesive systems Syntac and OptiBond FL (etch-and-rinse technique) and 

Clearfil SE Bond (self-etching) as controls. The samples were thermocycled after water storage for 21 days, after 1 

year and again after 3 years (2000 cycles between 5 and 55°C) and replicas were made before and after each thermocycling 

treatment (TC) for quantitative marginal analysis in the SEM. 

Results: In dentin, marginal adaptation showed no significant differences between all groups after the first TC. After 

one year of water storage and a second TC, the results for Prompt L-Pop (1999), Adper Prompt L-Pop/Tetric Ceram, 

and One-up Bond F Plus showed a statistically significant decrease of margin quality 1 (MQ1) score compared to the 

reference groups. When the all-in-one adhesives G-Bond, AQ-Bond, Hybrid Bond, and One-up Bond F Plus were used, 

the enamel margins of restorations showed lower percentages of “continuous margins” (p < 0.05) after 1 year of 

water storage and TC. Of the materials tested after 3 years of water storage and TC, only AQ Bond had a significantly 

lower MQ1 score. 

Conclusion: While all materials exhibited deterioration in the MQ1 quality score, the rate of deterioration varied, and 

the results show that different materials have different deterioration rates after initial vs long-term water storage. The 

deterioration along margins in dentin was not as extensive as predicted from other studies; however, the results from 

the enamel margins show that one-bottle all-in-one adhesives seem to be significantly affected by water storage. The 

results of this study suggest that the all-in-one adhesive group members perform very differently from each other: 

thus, data need to be explored further at the level of each different adhesive product 

Keywords: marginal quality evaluation, in vitro Class V restorations, adhesive system effectiveness. 


a Associate Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus 

Virchow Klinikum, Berlin, Germany. 

b Staff Scientist, Max Planck Institute of Colloids and Interfaces, Department of 

Biomaterials, Potsdam, Germany 



Reprint requests: Dr. Uwe Blunck, Charité-Universitätsmedizin Berlin, Dental 

School, Campus Virchow Clinic, Augustenburger Platz 1, 13353 Berlin, Germany. 

Tel: +49-30-450-562-673, Fax: +49-30-450-562-961. 

Adhesive systems are routinely used to improve the marginal 

seal of composite resin restorations at the interfaces 

with enamel and dentin. Bonding between enamel or 

dentin and the restorative composite must be sufficiently effective 

to resist the varying stresses to which a “typical” 

restoration is subjected. Such stresses include the polymerization 

shrinkage during composite placement as well as 

mechanical, thermal, and hydration stresses incurred in the 

oral environment due to normal use and wear. 25 

Available adhesive systems may be classified as dentinconditioning 

adhesive systems with selective acid etching 

on enamel, etch-and-rinse systems which necessitate phosphoric 

acid etching and rinsing of enamel/dentin prior to ap- 


Blunck/Zaslansky 

Table 1 Tested adhesive system/composite resin combinations 

Group Adhesive system Composite resin Adhesive manufacturer 

Multi-bottle systems Syntac Artemis Ivoclar Vivadent; Schaan, 

(control) 

Liechtenstein 

OptiBond FL Herculite XR Kerr; Danbury, CT, USA 

Clearfil SE Bond Clearfil AP-X Kuraray; Tokyo, Japan 

All-in-one Prompt L-Pop 1999 Tetric Ceram ESPE; Seefeld, Germany 

adhesive systems Prompt L-Pop 2000 Tetric Ceram ESPE 

with mixing Adper Prompt L-Pop Tetric Ceram 3M ESPE; St Paul, MN, USA 

Adper Prompt L-Pop Filtek Z250 3M ESPE 

Futurabond NR Grandio Voco; Cuxhaven, Germany 

One-up Bond F Estilite Tokuyama; Tokyo, Japan 

Xeno III Tetric Ceram Dentsply DeTrey; Konstanz, Germany 

Xeno III Dyract eXtra Dentsply DeTrey 

Xeno III Quixfil Dentsply DeTrey 

All-in-one AQ Bond Metafil CX Morita; Irvine, CA, USA 

adhesive systems G-Bond Gradia GC; Tokyo, Japan 

without mixing Hybrid Bond Metafil Morita 

iBond Charisma Heraeus Kulzer, Hanau, Germany 

tri-S bond Clearfil AP-X Kuraray 

plying multi-bottle or one-bottle adhesives, and self-etching 

systems that contain acid monomers which can condition 

both enamel and dentin simultaneously with no rinsing. 36 

Self-etching adhesive systems can be applied in two consecutive 

steps or as so-called all-in-one adhesives. The latter 

are available in two forms: those that require mixing and 

those that do not. 

The effectiveness of adhesive systems can be tested in 

vitro by bond strength measurements of various kinds, by 

penetration tests of Class V/II fillings with different substances, 

and by evaluating the margin quality of Class I/II/V 

or cylindrical fillings under a microscope. 17 In this study, visual 

inspection of discontinuities at the margins was performed 

using a scanning electron microscope (SEM), dedicated 

to the identification and quantification of dental margin 

qualities. 26 This method has several advantages, such 

as the high level of detail revealed and marked accuracy, allowing 

it to be used for evaluating the same margins at different 

times. This is particularly useful for testing the effects 

of water storage or stress on the same specimens. 

This paper considers the effectiveness of all-in-one adhesive 

systems in comparison to reference multi-bottle adhesive 

systems, as judged by evaluating the marginal integrity 

in dentin and enamel after different periods of water 

storage. The effects of short- vs long-term storage were exemplified 

by applying thermal stress in order to expose marginal 

degradation differences. This was used to study the 

state of the restoration margins at 3 weeks, 1 year and 3 

years, and consider some aspects of the dynamics of adhesive 

aging. 

MATERIALS AND METHODS 

This work reflects the current status of a large ongoing study. 

Teeth, anonymously collected following routine dental treatment, 

were stored in 0.1% thymol solution at room temperature 

prior to and during the experimental period. One hundred 

thirty-six caries-free extracted human anterior teeth 

were used, and typical Class V cavities were prepared with 

a diamond bur (diamond bur No. 838/314/014; Gebr. Brasseler; 

Lemgo, Germany) at high speed using water as a 

coolant. Oval preparations were a standard size: approximately 

4 mm high, 1.5 mm deep, and 3 mm wide (2 mm apical 

to the cementoenamel junction spanning across the CEJ 

and into enamel). The enamel portions were bevelled with a 

finishing diamond bur (Composhape H-15, Intensiv; Viganello-Lugano, 

Switzerland) and the cavosurface margins 

in dentin finished to a 90-degree angle with a finishing diamond 

(No. 8838/314/012, Gebr. Brasseler). The teeth were 

randomly divided into 17 groups of 8 teeth each. 

Each group of teeth was assigned to one of 17 treatments. 

These included 14 combinations of all-in-one adhesive 

system/composite resins and three multi-bottle adhesive 

systems (Syntac and OptiBond FL, etch-and-rinse technique, 

and Clearfil SE Bond, self-etching technique). The adhesives 

were all applied and restored with composite resin 

according to the manufacturer’s instructions as detailed in 

Table 1. In an attempt to ensure optimal performance of the 

adhesives, the composite used was generally that recommended 

by the adhesive manufacturer, although for some 

of the adhesives (Adper Prompt L-Pop and Xeno III), several 



composites were used. The composite resin was inserted in 

two increments (initially placed at the cervical margin), and 

each increment was light cured (Astralis 10 light-curing unit, 

Ivoclar Vivadent; Ellwangen, Germany) for 40 s. After finishing 

and polishing (Sof-Lex Pop-on Nr. 1981 SF/F/M/C 3M 

ESPE; St Paul, MN, USA), the teeth were returned to water 

storage for 21 days, followed by 2000 cycles of thermocycling 

(TC) between +5 and +55°C. 

Prior to and after TC, impressions were taken with a 

polyvinylsiloxane material (Silagum light body, DMG; Hamburg, 

Germany) and replicas of the restoration and surrounding 

tooth structures were produced. These were cast 

with an epoxy resin following precise manufacturer guidelines 

(Stycast 1266 Part A + B; Emerson and Cumming; Westerlo-Oevel, 

Belgium). Once fully cured, each replica was sputter-gold 

coated (SCD 030, Balzers Union; Balzers, Liechtenstein) 

in preparation for inspection by SEM. Similar impression 

and TC procedures were repeated after 1 year of water 

storage, and for 11 products also after 3 years. 

The effectiveness of each bonding system was assessed 

by evaluating the margins of the restorations at the 

dentin/composite and enamel/composite interface. Measurements 

were performed using a dedicated SEM (AMRAY 

1810, Amray; Bedford, MA, USA) and all replicas were viewed 

at a magnification of 200X, and classified according to the 

state of the margin in different areas in order to numerically 

quantify the marginal qualities, as detailed in Table 2. By 

using this method, each segment of the tooth/restoration interface 

was imaged and ranked according to defined quality 

criteria. These were then converted into percentage of the 

total margin length, in dentin and enamel independently. 

Statistical evaluation was performed using an SPSS statistical 

software package (SPSS Software; München, Germany). 

Within each sample group, significant differences 

were determined using the nonparametric Wilcoxon test. For 

comparison between the different treatment groups, the 

nonparametric Kruskal-Wallis test was used followed by Bonferroni 

adjustment. The statistics were calculated for the parameter 

margin quality 1 (MQ1 = “excellent” or “continuous” 

margin). Origin 7.0 SR0 (Originlab; Northampton, MA, USA) 

was used for the weighted regression and Microsoft Excel 

(2000) was used to determine the slopes between MQ1 

rankings at different stages of the experiment. 

RESULTS 

The results of the 14 test groups were compared with those 

of the 3 reference multi-bottle adhesives OptiBond FL, Syntac, 

and Clearfil SE Bond. Figure 1 is a box-and-whiskers plot 

of the marginal quality MQ1results determined for the enamel 

margins, depicting the median, 25 and 75 percentiles. 

The main result seen here is that after 1 year of water storage 

(Fig 1a) and following a second TC, a reduction (significant 

at p < 0.05) in the amounts of “continuous margins” 

(MQ1) is seen for G-Bond, AQ-Bond, Hybrid Bond, and Oneup 

Bond F Plus. No significant difference was found between 

any other of the groups and the reference adhesives. After 

3 years of water storage and a third TC, only AQ Bond had a 

substantially lower MQ1 score (p < 0.05). 

Table 2 Criteria for the marginal analysis in the SEM 

Margin 

quality 

Definition 

1 Margin not or hardly visible, no or slight marginal 

irregularities*; no gap 

2 No gap but severe marginal irregularities* 

3 Gap visible (hairline crack up to 2μm, no marginal 

irregularities* 

4 Severe gap (more than 2μm), slight and severe 

marginal irregularities* 

* The term "marginal irregularities" refers to porosities, marginal 

restoration fracture, or bulge in the restoration 

Figure 2 shows the MQ1 results that were obtained for 

each product in dentin following each of the three TC treatments. 

Following the first TC (Fig 2a), no statistically significant 

differences were found for any of the groups. The TC after 

1 year of water storage (Fig 2b) revealed a decrease in 

MQ1 for Prompt L-Pop in the 1999 version, Adper Prompt L- 

Pop/Tetric Ceram, and One-up Bond F Plus (p < 0.05). After 

three years of water storage and a 3rd TC both Prompt L-Pop 

(1999) and Adper Prompt L-Pop/Tetric Ceram were found to 

have substantially lower MQ1 scores than the reference 

groups (p < 0.05). Data for One-up Bond F Plus, G-Bond, AQ- 

Bond, Hybrid Bond, and tri-S Bond are missing for three 

years, as these materials were not available for the full duration 

of the present study. 

To better understand the dynamics of the results presented 

in Fig 2 and to obtain insights into the effects of TC 

and water storage, plots were produced of MQ1 for each 

group before and after TC at 21 days (T1 and T2), after 1 year 

of water storage (T3 and T4) and after 3 years of water storage 

(T5 and T6). Only the plots for the reference multi-bottle 

products are shown as examples in Fig 3. Each data point 

(T1-T6) represents the median MQ1 values with the corresponding 

error bars that are the standard error of the mean 

(SE). It must be emphasized that in these plots, the time intervals 

between the data points are not equal. The trends of 

the T1-T2, T2-T4, and T4-T6 segments were calculated in 

each graph, because the effects of water storage alone (segment 

T2-T3 after 1 year and segment T4-T5 after 2 additional 

years) were too small to be directly and reliably visualized. 

Thus, the purpose of TC was to challenge the bonds 

of the restorations in order to test the marginal integrity. Further 

analysis was then used to explore the joint effects of TC 

after the different water storage periods. 

The T1-T2, T2-T4, and T4-T6 slopes as well as the statistical 

significance (p) of the difference between each pair of the 

corresponding MQ1 values (obtained with the nonparametric 

Wilcoxon rank test) are presented in Table 3, columns A to 

F (shown as 1 st water storage [WS] vs 1 st TC, 1 st TC vs 2 nd TC, 

2 nd TC vs 3 rd TC). We also calculated trends in the overall adhesive 

effectiveness by fitting linear regression lines (error 



0 

20 

40 

60 

80 

100 % 

+ 

Syntac 

OptiBond FL 

Clearfil SE Bond 

a. 

MQ1 

results after 

2 nd TC 

enamel 

+ 

+ 

* 

* 

* 

Prompt L-Pop 1999 


Adper Prompt L-Pop / Tetric Ceram 

Adper Prompt L-Pop / Filtek Z250 

Xeno III / Quixfil 

Xeno III / Tetric Ceram 

Xeno III / Dyract eXtra 

Futurabond NR 

One-up Bond F Plus 

AQ Bond 

iBond 

G-Bond 

Hybrid Bond 

tri-S bond 

+ 

Syntac 

OptiBond FL 


b. 

MQ1 

results after 

3 rd TC 

enamel 

+ 





0 

20 

40 

6 

0 

80 

* 

100 % 



AQ Bond 

iBond 

Fig 1 Results of marginal quality 

1 in % relative to the enamel margin 

length in Class V cavities for 

self-etching adhesive systems 

after (a) 1-year water storage and 

a 2nd TC and (b) after after 3- 

year water storage and a 3rd TC 

(o and + = outliers, * = statistically 

significantly different compared 

to Syntac, Opti Bond FL, 

and Clearfil SE Bond, p < 0.05). 

weighted by the SE) through the six MQ1 data points for every 

product. The slopes of these regression lines, as well as the 

95% confidence intervals and r 2 values are also shown in 

Table 3 (columns I to L), and they provide an overall estimate 

of the trend for the deterioration of the MQ1 results for each 

product. A general linear deterioration was observed for all 

groups (see example plots in Fig 3), which shows that the deterioration 

rate is not consistent over time. Furthermore, for 

all the products, the overall trend (column I) only occasionally 

corresponds to the trend of the intermediate segments 

(columns A, C, E, and G in Table 3). 

Finally, to better understand how well the data from the 

first year can be used to predict the trend in the performance 

of each product over a period of 3 years, the trends of T1 - 

T4 were calculated and used to derive a percent deviation 

estimate relative to the regressed overall trend (the difference 

divided by the slope of the overall trend as %, shown in 

Table 3, column M). Note that for some of the products (Opti- 

Bond FL, AQ Bond, Prompt L Pop 2000, Adper Prompt L Pop, 

and Xeno III) a reasonable (≤ 10%) prediction was found, 

while for others, deviations of 20%, 30% or even 40% exist. 

DISCUSSION 

Effectiveness of adhesive systems can be generally judged 

by the marginal adaptation of composite resin restorations 

at the interface with the tooth substrate. Marginal adaptation 

is affected by many different parameters. These might 

be greatly influenced by the inherent properties of the 

restorative material, such as shrinkage and shrinkage 

stress, 24 the chemistry of the adhesive system used, the size 



0 

20 

40 

60 

80 

100 % 

Syntac 

Optibond FL 


a. 

MQ1 

results after 

1 st TC 

dentin 

+ 

Prompt L-Pop (1999) 

Prompt L-Pop (2000) 






Futurabond NR 

One Up Bond F Plus 

AQ Bond 

iBond 

Hybrid Bond 

G-Bond 

tri-S bond 

Syntac 

OptiBond FL 


b. 

MQ1 

results after 

2 nd TC 

dentin 

* 

* 

* 








Futurabond NR 

One-up Bond F-Plus 

AQ Bond 

iBond 

Hybrid Bond 

G-Bond 

tri-S bond 

Fig 2 Marginal quality 1 results 

in % of the dentin margin length in 

Class V cavities for all-in-one adhesive 

systems after (a) 21 days of 

water storage and a 1st TC, after 

(b) 1 year of water storage and a 

2nd TC, and (c) after after 3 years 

of water storage and a 3rd TC (o 

and + = outliers, * = statistically 

significantly different compared to 

Syntax, OptiBond FL, and Clearfil 

SE Bond p < 0.05). 

c. 

MQ1 

results after 

3 rd TC 

dentin 

0 

20 

40 

+ 

6 

0 

+ 

80 

* 

* 

100 % 

Syntac 

OptiBond FL 








AQ Bond 

iBond 

of the cavity, the c-factor, 9 the insertion technique, and the 

polymerization protocol. 1 

In this study, a high resolution quantitative marginal 

analysis method was used to evaluate the marginal adaptation 

of composite resin restorations over a long period of water 

storage followed by TC. This quantification method relies 

on imaging of precision replicas of restored teeth with a 

scanning electron microscope, followed by quantitative quality 

analysis of the entire margin length. The replica technique 

is non-destructive to the natural-tooth samples; hence, the 

margins can be assessed and marginal defects detected 

and compared at different times, as well as after applying 

different stresses to the tooth specimens. The high sensitivity 

of this method, due to the SEM's excellent detail reproduction, 

is a great advantage for the evaluation of such 

bonding of adhesive systems. 4,26 

The results (Figs 1 and 2) show a distribution of the MQ1 

results of the restoration margins at different stages of the 



[% MQ1] 

100 

95 

a. 

90 

85 

Optibond FL 

80 

75 

T1 T2 T3 T4 T5 T6 

[% MQ1] 

100 

95 

b. 

90 

85 

Syntac 

80 

75 

T1 T2 T3 T4 T5 T6 

c. 

[% MQ1] 

100 

95 

90 

85 

80 

75 


T1 T2 T3 T4 T5 T6 

Fig 3 Median MQ1 values in % of entire margin length 

in dentin with error bars indicating the standard error of 

the mean for the multi-bottle reference materials (a) Opti 

Bond FL, (b) Syntac and (c) Clearfil SE Bond at the six 

evaluation stages T1 (after 21 days’ water storage), T2 

(after 1st TC), T3 (after 1 year of water storage), T4 (after 

2nd TC), T5 (after 3 years of water storage) and T6 (after 

3rd TC). Black lines: regression lines weighted by the corresponding 

standard error; dotted lines: 95% confidence 

intervals. 

study, but overall the scores are quite high, perhaps due to 

the fact that the deterioration is generally quite minimal. 

Further examination of the present data allows creating a 

quasi-dynamic perspective of the deterioration rate of the 

restorations (Fig 3 and Table 3). Thus it is seen that there is 

a general negative trend in the MQ1 values, when these are 

determined after water storage and/or thermocycling (TC). 

Clearly, the specific state of the bond between each 

restorative and the tooth is not easily determined by any surface-evaluation 

method, particularly following long-term water 

storage. The decision was thus made to use TC to induce 

mild stress to every tooth-restoration interface in order to better 

reveal its state as determined by the marginal quality evaluation. 

As can be seen in Table 3, the effect of TC is not constant 

during early vs late (> 1 year) water storage, and this is 

attributed to the differences in the adhesive stability in water. 

A number of publications have dealt with the effects of 

similar long-term water storage beyond 2 years. 2,3,7,16,22, 

23,27 To the best of our knowledge, however, none have managed 

to produce high-resolution long-term data mapping the 

marginal quality deterioration on the same samples. 

Despite the fact that the cavity dimensions were standardized, 

the amount of stress induced to the interface of 

each restoration probably varied considerably. This might 

be due to the large variations in the coefficients of thermal 

expansion of each restorative 28,29 or possibly due to tooth 

variability. Be that as it may, because the manufacturer-recommended 

composites were used, it was assumed that the 

conditions were optimal for each adhesive, and that the 

best performance was obtained. It remains to be seen if other 

combinations of composite/adhesive deliver improved 

long-term results. Possibly, a standard composite restorative 

should be used for such tests in the future in order to 

better compare the effectiveness of the investigated adhesives. 

The importance of the effect of the composite resins 

can clearly be seen in the groups of Adper Prompt L-Pop and 

Xeno III, where large differences in MQ1 values and slopes 

are seen for the same adhesive. Note however, that while 

Adper Prompt L-Pop in combination with Tetric Ceram 

showed a statistically significant decrease in MQ1 compared 

to the results obtained with Filtek Z250, all three 

combinations with Xeno III (Dyract XP, Quixfil, and Tetric Ceram) 

revealed no statistically significant differences in marginal 

integrity. We therefore conclude that these adhesives 

react differently to composite resins with higher polymerization 

shrinkage stress values. 

Both in vitro 6,7,10,11 and in vivo studies 8,12,13,35,37 have 

shown that multi-bottle multi-step adhesive systems such as 



Table 3 Slopes of regression lines and statistical significance (p) of results from different evaluation stages after water storage (WS) and thermocycling (TC): 

columns A + B = 1 st WS vs 1 st TC, columns C + D = 1 st TC vs 2 nd TC, columns E + F = 2 nd TC vs 3 rd TC, columns G + H = 1 st WS vs 2 nd TC. Columns I to L show the 

slope for the regression lines for all data points of one group, r 2 -values, lower (LCI) and upper confidence intervals (UCI). The last column shows the percentage 

of deviation between the slopes of the overall regression lines (column I) and the regression lines between 1 st and 2 nd TC (column C). n.a. = not analyzed (data 

were not available after 3 years of water storage). Column M is the percent deviation calculated by the formula [100*(I col I - col G I/col I)] where col I and col 

G refer to values in columns I and G, resp. 

A B C D E F G H I J K L M 

1 st WS vs 1 st TC 1 st TC vs 2 nd TC 2 nd TC vs 3 rd TC 1 st WS vs 2 nd TC r 2 LCI UCI % 

slope p slope p slope p slope p Deviation 

Syntac / 

Artemis -2.36 0.173 -0.73 0.028 -0.53 0.028 -1.27 0.028 -0.97 0.91 -1.99 0.05 30.93 

OptiBond FL / 

Herculite XR -1.80 0.018 -1.26 0.069 -1.97 0.017 -1.44 0.017 -1.56 0.98 -2.65 -0.48 7.69 

Clearfil SE Bond / 

Clearfil AP-X 0.00 0.109 -4.33 0.018 -2.88 0.012 -1.53 0.018 -2.50 0.89 -3.41 -1.60 38.80 

Prompt L-Pop 1999 / 

Tetric Ceram -6.11 0.018 -21.99 0.012 -3.40 0.012 -16.70 0.012 -13.06 0.95 -15.45 -10.68 27.87 

Prompt L-Pop 2000 / 

Tetric Ceram -6.94 0.018 -4.01 0.093 -3.71 0.012 -4.99 0.012 -4.52 0.98 -5.80 -3.25 10.40 

Adper Prompt L-Pop / 

Tetric Ceram -6.23 0.018 -10.51 0.012 -6.17 0.012 -9.08 0.012 -8.55 0.98 -10.30 -6.81 6.20 

Adper Prompt L-Pop / 

Filtek Z250 -3.32 0.018 -3.69 0.012 -1.55 0.012 -3.56 0.012 -2.95 0.97 -3.83 -2.06 20.68 

Xeno III / 

Tetric Ceram -0.89 0.068 -2.13 0.043 -0.92 0.018 -1.72 0.028 -1.35 0.91 -2.78 0.07 27.41 

Xeno III / 

Dyract eXtra -2.61 0.043 -0.40 0.043 -0.84 0.012 -1.13 0.043 -1.09 0.92 -2.80 0.62 3.67 

Xeno III / 

Quixfil -1.77 0.138 -2.72 0.028 n.a. n.a. -2.40 0.028 -2.07 0.96 -4.65 0.51 15.94 

Futurabond NR / 

Grandio -3.83 0.028 -1.32 0.018 n.a. n.a. -2.15 0.018 -2.21 0.94 -4.34 -0.09 2.71 

One-up Bond F Plus/ 

Estilite -6.43 0.012 -11.49 0.012 n.a. n.a. -9.80 0.012 -6.65 0.77 -12.77 -0.53 47.37 

AQ Bond / 

Metafil CX 0.00 0.109 -2.66 0.401 -1.60 0.069 -1.77 0.028 -1.63 0.96 -2.36 -0.90 8.59 

Hybrid Bond / 

Metafil -4.31 0.018 -1.83 0.018 n.a. n.a. -2.66 0.018 -2.62 0.95 -4.94 -0.30 1.53 

iBond / 

Charisma -0.95 0.043 -3.07 0.028 -0.95 0.012 -2.36 0.028 -1.83 0.95 -2.99 -0.68 28.96 

G-Bond / 

Gradia -4.22 0.012 -7.16 0.012 n.a. n.a. -6.18 0.012 -4.61 0.78 -8.44 -0.78 34.06 

tri-S Bond / 

Clearfil AP-X -6.20 0.012 -3.12 0.012 n.a. n.a. -4.15 0.012 -3.90 0.93 -6.03 -1.76 6.41 



a. 

21 days of WS vs. 1st TC 

multi-bottle adhesives 

all-in-one adhesiv es w ith mixing 

all-in-one adhesiv es w ithout mixing 

-25 -20 -15 -10 -5 0 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

AQ Bond 



iBond 


OptiBond FL 

Syntac 



Futurabond NR 

G-Bond 

Hybrid Bond 


tri-S Bond 




b. 

1st TC vs. 2nd TC 

multi-bottle adhesives 

all-in-one adhesiv es w ith mixing 

all-in-one adhesiv es w ithout mixing 

-25 -20 -15 -10 -5 0 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 

* 


Syntac 

OptiBond FL 

Futurabond NR 

Hybrid Bond 


AQ Bond 


iBond 

tri-S Bond 




G-Bond 




Fig 4 Ranked slopes of regression 

lines through MQ1 values 

in dentin for each product (a) 

after 21 days of water storage 

vs 1 st TC (column A in Table 3) 

and (b) 1 st TC vs 2 nd TC (column 

C in Table 3). * denotes 

stopes that were determined 

between MQ1 median values 

that are statistically different 

with p < 0.05 (Wilcoxon test). 

OptiBond FL and Syntac in combination with the etch-andrinse 

technique and the multi-step self-etching adhesive 

Clearfil SE Bond are reliable adhesives even after long-term 

usage. For this reason, these three products were used as 

reference materials in this study. They also provide to some 

extent a means to calibrate the present results with other 

studies. With the quasi-dynamic trends, it is possible to rank 

the different adhesives according to their rate of deterioration 

(as shown for mainly after TC) after 21 days or 1 year in 

water (see example Figs 4a and 4b). This ranking differs for 

the two water storage periods, which can be attributed to the 

specific properties of each adhesive, which lead to differences 

in bond quality and rates of degradation. 

The working assumption of this study was that better performance 

of any adhesive group would be associated with 

the highest (least negative) slope of MQ1 deterioration (column 

I in Table 3). These slope values are different from the 

slopes of the individual segments 1st WS vs 1st TC and 1st 

vs 2nd TC, and thus the rate of deterioration of the bonds 

might vary substantially over time. As seen in Figs 4a and 4b, 


Blunk/Zaslansky 

many of the products, change the rank between the initial 

water storage period, as compared with the rank after the 

first year . We are aware that such ranking might be of limited 

use for predicting clinical performance; therefore, clinicians 

and manufacturers might need to define criteria for 

“adequate performance”, not “better performance”. Clearly 

such long-term effects need to be considered in addition to 

operation skill and experience, 15,21 both of which are difficult 

to account for, therefore consequences of these findings 

necessitate further investigations. 

The marginal analysis centered on the quantitative evaluation 

of MQ1 (“excellent” or “continuous” margin) as a 

measure for marginal integrity. It has recently been shown 

that such an evaluation provides a good indicator for the 

ability of an adhesive system to compensate for the shrinkage 

of composite resins during polymerization, as compared 

to bond strength tests. 17 The extent to which the present in 

vitro results correspond to in vivo data of quantitative marginal 

analysis of Class V fillings is not obvious, especially as 

there are reports showing that such data are unable to predict 

clinical outcome. 17 Nevertheless, results of this study 

and trend analysis provide an additional means of determining 

objective and standard measures of the physical attributes 

of any combination of adhesive system and composites. 

It therefore remains to be seen just how such details 

match the outcomes of clinical investigations. It is worthwhile 

to note that other studies have evaluated the marginal 

quality using stress induced by mechanical loading. 12,13 

The method employed in this study has the advantage that 

TC induces precise and repeatable stress (assuming the coefficient 

of thermal expansion of the composites stays constant), 

and this concept was used to provide more information 

about the effects of water storage at short and long intervals. 

The present results are based on SEM evaluation of the 

percentage of the different marginal qualities, calculated in 

relation to the entire margin length in dentin or enamel independently. 

It has been shown that when the same operator 

evaluates the same specimens twice, the difference between 

the results is in the range of 4%, 26 whereas when two 

trained operators evaluate the same specimens, the differences 

can reach 10% to 20%. 18 Therefore, all specimens in 

this study were prepared and evaluated by the same operator. 

It is interesting to note that for most of the products not 

displaying a large discrepancy between the initial and intermediate 

MQ1 values, the first-year data provide only a moderate 

predictor for the longer term trend of deterioration. 

Therefore, initial predictors of restorative success have limited 

applicability, and more data over long periods of time 

are needed. This is unavoidable even in an in vivo setting, 

and is important especially when both manufacturers and 

clinicians want to know as early as possible which is the best 

product. It is, of course, conceivable that storage at higher 

temperatures might allow faster answers to these questions. 

All-in-one adhesives are rather user friendly; however, certain 

indicators have suggested reduced performance that 

might be associated with their usage. Compared with twostep 

self-etching or etch-and-rinse adhesive systems, lower 

bond strength values were reported. 5,14,19,20 It has also 

been shown that permeable membranes develop after curing 

due to a high hydrophilicity, which allows water movements 

through the all-in-one adhesive layer. 30 Sites of incomplete 

water removal and subsequent suboptimally polymerized 

resins 31 have been described and termed “water 

trees”. All these might contribute to extensive degradation 

of the adhesive layer, 7,32 but conclusive findings have not 

been confirmed. The most recent (to date) one-bottle all-inone 

adhesives appear to be susceptible to phase separation 

after dispensing the complex mixture of hydrophobic and hydrophilic 

components, 34 and this also is assumed to contribute 

to bond degradation. 33 

This study has presented preliminary results of short- and 

long-term water storage effects combined with thermocycling 

for control and 14 all-in-one adhesive/composite treatments. 

The results show that overall, few if any differences 

are found in vitro between the tested products and the reference 

materials. Furthermore, based on a quality estimate 

associated with the marginal integrity, it has been shown 

that early deterioration rates (up to 1 year) can only sometimes 

be used as estimates for the rate of bond degradation 

over a period of 3 years. Indeed, it seems that deterioration 

rates due to storage in water are not dependent on the class 

(or generation) of the adhesive: large differences in deterioration 

rates seem to exist between different products, and 

these are probably associated with the details of the specific 

chemistry. Additional studies are still needed in order to 

elucidate to what extent – and in which product – deterioration 

is critical. These should then be correlated with clinical 

studies so that decisive conclusions can be drawn . 

It appears that the effects of long-term water storage may 

not be as detrimental as usually assumed, if indeed the marginal 

integrity estimates are appropriate measures of the 

quality and effectiveness of recent generations of dental adhesives. 

A statistically significant decrease in the amount of 

MQ1 was only found in 3 out of 14 tested all-in-one adhesives 

after 1 year water storage. However, in enamel, the 

marginal analysis revealed fewer “continuous margins” than 

the control groups for G-Bond, AQ Bond, Hybrid Bond, and 

One-up Bond F Plus, and this was already observed after 1 

year of water storage. 

As new results of clinical evaluations emerge, and with a 

growing body of data from in vitro measurements, it is hoped 

that a clearer understanding of the long-term effects of the 

use of these systems will emerge, thus providing an improved 

guide for clinical judgement. 

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15. Giachetti L, Russo DS, Bertini F, Pierleoni F, Nieri M. Effect of operator skill 

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31. Tay FR, Pashley DH, Yoshiyama M. Two modes of nanoleakage expression 

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32. Tay FR, Pashley DH. Water treeing--a potential mechanism for degradation 

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Y, Inoue S, Peumans M, Suzuki K, Lambrechts P, Van Meerbeek B. 

Monomer-solvent phase separation in one-step self-etch adhesives. J Dent 

Res 2005;84:183-188. 

35. Van Meerbeek B, Perdigao J, Lambrechts P, Vanherle G. The clinical performance 

of adhesives. J Dent 1998;26:1-20. 

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Landuyt K, Lambrechts P, Vanherle G. Buonocore memorial lecture. Adhesion 

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Dent 2003;28:215-235. 

37. van Meerbeek B, Kanumilli P, de Munck J, Van Landuyt K, Lambrechts P, 

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Clinical relevance: Quantitative in vitro long-term measurements 

of margin integrity help to better understand 

the performance of composite resin restorations in the 

clinic. In combination with clinical studies this should 

provide a deeper understanding of the adhesive failure 

an which remains enormous challenge for dentists. 


Clinical Bonding of a Single-step Self-etching Adhesive 

in Noncarious Cervical Lesions 

Jan WV van Dijken a /Karin Sunnegårdh-Grönberg b /Ebba Sörensson b 

Purpose: The aim of this study was to evaluate the clinical retention to dentin of a single-step self-etching adhesive 

system. 

Materials and Methods: A total of 133 Class V restorations were placed with the self-etching primer Xeno III and a 

resin composite (Tetric Ceram) or a polyacid-modified resin composite (Dyract AP) in noncarious cervical lesions without 

intentional enamel involvement. The restorations were evaluated at baseline and then every 6 months during a 2- 

year follow-up. Dentin bonding efficacy was determined by the percentage of lost restorations. 

Results: During the 2 years, 130 restorations could be evaluated. The cumulative loss rate at 2 years was 7.7%, with 

no significant differences between the two restorative materials. The self-etching adhesive fulfilled the 18-month full 

acceptance ADA criteria. 

Conclusion: The single-step self-etching adhesive showed acceptable clinical retention rates to dentin surfaces during 

the evaluation period independent of restorative material used. 

Keywords: adhesion, clinical, cervical, dental material, etch, resin, restoration, self-etching. 


a Professor, Department of Odontology, Dental School Umeå, Umeå University, 

Umeå, Sweden. 

b Assistant Professor, Department of Odontology, Dental School Umeå, Umeå University, 

Umeå, Sweden. 



Reprint requests: Prof. Jan WV van Dijken, Department of Odontology, Dental 

School Umeå, Umeå University , 901 87 Umeå, Sweden. Tel: +46-90-785-6034, 

Fax: +46-90-770-580. e-mail: Jan.van.Dijken@odont.umu.se 

The introduction of primers containing amphiphilic monomers 

– dissolved in solvents such as water, acetone, or 

alcohol to promote wetting of the dentin and replace water 

– changed dentin bonding to a more reliable clinical procedure. 

These primers infiltrate the nanospaces of the collagen 

network, caused by the etching procedure, and create 

after polymerization an entangled molecular mesh with the 

collagen fibrils. 4 A high micromechanical bond to the dental 

tissue can be obtained by formation of the so-called hybrid 

layer. In the multistep etch-and-rinse systems, clinical success 

is partly operator related. The etching and primer application 

steps are critical in this approach. Bonding procedures 

not involving phosphoric acid etching, such as the selfetching 

adhesives, were introduced in the 90s to simplify the 

adhesive procedure and decrease the technique sensitivity 

of the etch-and-rinse systems. The simultaneous self-etching 

and primer infiltration makes these systems more user 

friendly, eliminating the risk of over etching and over drying. 

Today, there are two self-etching systems. The two-step selfetching 

adhesives have a separate priming step with more 

hydrophilic monomers and a more hydrophobic bonding 

step. In the all-in-one or one-step self-etching adhesives, one 

liquid containing all the components for etching, priming, 

and bonding is applied to the dental tissues. Earlier mild selfetching 

adhesives showed etching patterns of the enamel 

which were not adequate for clinical retention, and some 

manufacturers recommended the adjunctive use of phosphoric 

acid when bonding to enamel. 5 Incompatibility with 

autocuring resin composites and permeability to water 

movement after polymerization have been reported for the 

first all-in-one adhesives. 14,15 Newer self-etching adhesives 

contain more aggressive etchants and showed higher tensile 

bond strength compared to established dentin bonding 

agents. 7 The aim of this study was to investigate the clinical 

dentin bonding effectiveness of a new one-step self-etching 

adhesive in combination with a resin composite material or 

a polyacid resin-modified resin composite in noncarious cer- 


van Dijken et al 

Fig 1 Relative cumulative loss rates 

(%) of the Xeno III bonding system in 

combination with the two restorative 

materials (Tetric Ceram, Dyract AP). 

vical lesions. The hypothesis tested was that the polyacid 

resin-modified resin composite would show better clinical retention. 


A total of 133 Class V restorations were placed in 57 patients 

(32 men and 25 women) with a mean age of 61.5 years 

(range 43 to 84), for whom treatment of noncarious cervical 

lesions was indicated. All restorations were placed in dentin 

lesions without any intentional enamel involvement, by one 

experienced operator familiar with adhesive dentistry. Fortyfour 

restorations were placed in anterior teeth, 55 in premolars 

and 32 in molars. Fifty-nine restorations were made 

in the maxillary arch and 74 in the mandibular. A single-step 

self-etching primer (Xeno III, Dentsply/DeTrey; Konstanz, 

Germany; lot nr 0206001237) was evaluated in combination 

with two different restorative resinous materials, a hybrid 

resin composite (Tetric Ceram, Ivoclar/Vivadent; 

Schaan, Liechtenstein; lot E17820) and a polyacid-modified 

resin composite (Dyract AP, Dentsply/DeTrey; batch nr 

0203001190). Liquid A of the two-part adhesive system 

contains water, ethanol, HEMA, UDMA and BHT (2,6-di-tertbutyl-p 

hydroxyl toluene) and nanofiller. Liquid B contains 

UDMA, CQ, EPD (p-dimethylaminoethyl benzoate) and two 

patented monomers Pyro-EMA (tetramethacryloxyethyl pyrophosphate 

and PEM-F (pentamethacryloxyethyl cyclophosphazene 

monofluoride). 

The operative field was isolated with cotton rolls and a 

saliva suction device. Before conditioning, the lesions were 

cleaned of plaque and/or saliva if necessary. The adjacent 

gingiva was retracted by gingival retraction instruments or 

matrix bands when necessary to secure unrestricted contamination-free 

access to the field. No bevel was placed. Application 

of the primer was performed according to the manufacturers’ 

instructions. After mixing, the primer was applied 

for 20 s, carefully air dried for some seconds to remove 

the solvent, taking care not to thin the primer layer. The layer 

was then light cured for at least 10 s (Astralis 7, HP curing 

mode; Ivoclar/Vivadent). Sixty-five restorations were 

made at random with the polyacid resin-modified resin composite 

and 68 with a high-viscosity resin composite restorative 

material. The restoratives were applied in most cases in 

two increments using selected composite instruments (Hu 

Friedy; Leimen, Germany) and light cured. All participants 

were informed about the material and the follow-up evaluations 

according to the rules at the Dental School Umeå. The 

restorations were evaluated at 6, 12, 18, and 24 months using 

slightly modified USPHS criteria. 3,5 Only the retention 

evaluations are reported here. Postoperative sensitivity was 

registered. Descriptive statistics were used to present the results. 

Cumulative retention failures were calculated by dividing 

the number of lost restorations at the recalls by the 

total number evaluated at the respective recall. Differences 

in distribution of the ratings between the adhesive systems 

for the investigated variables were statistically analyzed with 

the binomial test for independent samples and intraindividual 

comparisons of the 2 materials with Friedman’s two-way 

analysis of variance. 13 

RESULTS 

At the end of the follow-up, 130 restorations could be evaluated. 

One patient with three restorations was not able to attend 

the 2-year recall. No recurrent caries was observed or 

postoperative sensitivity reported. Ten lost restorations 

(7.7%) were observed during the 2-year follow-up, resulting 

in relative cumulative failure frequencies for all restorations 

at 6, 12, 18, and 24 months of 0.8%, 3.1%, 6.9%, and 7.7%, 

respectively. The failure frequencies for the restorations with 

Tetric Ceram at the four evaluations were 0%, 0%, 5.9%, and 

7.4%, and for Dyract AP restorations 1.6%, 6.5%, 8.1%, and 

8.1%, respectively; the differences were not statistically significant 

(Fig 1). 


van Dijken et al 

DISCUSSION 

The rapid progression of adhesive materials during the last 

20 years has resulted in a situation where many adhesive 

systems have been replaced by modified successors which 

were claimed to be better without clinical validation. Clinical 

trials have been limited in number since they require several 

years of regular recalls. Enamel-resin bonds produced after 

acid etching with phosphoric acid have proven satisfactory 

and stable over time. 2,5,6 Adhesion to dentin, on the other 

hand, has been difficult to achieve because of the substrate’s 

wet nature. The efficacy of dentin bonding can be 

demonstrated in cervical abrasion/erosion lesions without 

involvement of the contiguous enamel. These surfaces are 

ideal to test clinical dentin bonding because they are widely 

available. 12 Therefore, no enamel bevel was made in the 

study and care was taken not to involve the enamel surface 

contiguous with the lesions during the etching-priming step. 

However, many of the lesions still contained a small enamel 

margin in the incisal area, and the evaluation of clinical 

retention to only dentin tissue was therefore not 100%. At 

the end of the two years, the recall rate was high (130/133). 

The retention rate for the adhesive system was 92.3%. 

Türkün recently reported a 96% retention rate after one year 

for the same adhesive. 16 For provisional acceptance, the latest 

guidelines of the American Dental Association (Dental 

and enamel adhesive materials: ADA, Council on Dental Materials, 

Instruments, and Equipment, 1994) for submission 

of dentin and enamel adhesive materials require that no 

more than 5% of the restorations have been lost and not 

more than 5% of the restorations may show microleakage at 

the 6-month recall. To obtain full acceptance, the cumulative 

incidence of clinical failures in each of two independent clinical 

studies has to be lower than 10% lost restorations and 

10% microleakage after 18 months. The dentin retention 

rates for the tested adhesive were 3.1% and 6.9% at 6 and 

18 months, respectively, fulfilling the ADA guidelines for 

enamel-dentin adhesive systems. There were no significant 

differences in clinical retention rates between the restorations 

placed with the resin composite or the polyacid-modified 

resin composite. The hypothesis was therefore not accepted. 

Kemp-Scholte et al 8 showed that materials with lower 

elasticity modulus can act as an elastic buffer, which relieved 

contraction stresses and improved marginal integrity. 

Since most polyacid-modified resin composites include 

resins with a modulus of elasticity value between those of 

resin composite and glass-ionomer cement, these materials 

may work as a stress-breaking barrier between the tooth and 

the composite. 1 A significantly better adaptation was observed 

with the SEM replica technique for a polyacid-modified 

resin composite/resin composite sandwich technique 

compared to resin composite only restorations. 9 However, 

the same authors could not show any clinical evidence for 

the interfacial adaptation results observed by SEM. No significant 

statistical or clinical differences were observed between 

the two techniques during 3- and 9-year periods. 10,11 

The polyacid-modified resin composite tested in the present 

study has a modulus of elasticity value close to that of resin 

composite materials, which may partly explain why no differences 

were observed (personal communication, E. Asmussen). 

CONCLUSION 

It can be concluded that the single-step self-etching adhesive 

showed acceptable clinical retention rates during the 

evaluation period, independent of restorative material used. 

ACKNOWLEDGMENTS 

This study was supported in part by the County Council of Västerbotten 

and Dentsply DeTrey, Konstanz, Germany. 

REFERENCES 

1. Attin T, Vataschki M, Hellwig E. Properties of resin-modified glass-ionomer 

restorative materials and two polyacid-modified resin composite materials. 

Quintessence Int 1996;27:203-209. 

2. de Munck J, van Landuyt K, Peumans M, Poitevin A, Lambrechts P, Braem M, 

van Meerbeek B. A critical review of the durability of adhesion to tooth tissue: 

methods and results. J Dent Res 2005;84:118-132. 

3. Dijken van JWV. A clincial evaluation of anterior conventional, microfiller and 

hybrid composite resin fillings. A six year follow up study. Acta Odont Scand 

1986;44:357-367. 

4. Dijken van JWV. Multi-step versus simplified enamel-dentin bonding systems- 

Réalités Cliniques 1999;10:199-222. 

5. Dijken van JWV. Durability of new restorative materials in Class III cavities. J 

Adhes Dent 2001;3:65-70. 

6. Frankenberger R, Krämer N, Petschelt A. Long term effect of dentin primers 

on enamel bond strength and marginal adaptation. Oper Dent 2000;25:11- 

19. 

7. Gernhardt CR, Biesecke G, Schaller HG. Tensile bond strength of a self-conditioning 

dentin adhesive system in vitro [abstract 338]. J Dent Res 

2003;82:B 55. 

8. Kemp-Scholte CM, Davidson CL. Marginal integrity related to bond strength 

and strain capacity of composite resin restorative systems. J Prosth Dent 

1990;64:658-664. 

9. Lindberg A, Dijken van JWV, Hörstedt P. Interfacial adaptation of a Class II 

polyacid-modified resin composite/ resin composite laminate restoration in 

vivo. Acta Odont Scand 2000;58:77-84. 

10. Lindberg A, van Dijken JWV, Lindberg M. A 3-year evaluation of a new open 

sandwich technique in class II cavities. Am J Dent 2003;15:33-36. 

11. Lindberg A, van Dijken JWV, Lindberg M. 9-year evaluation of a poly-acid-modified 

resin composite open sandwich technique in class II cavities. J Dent 

2007;35:124-129. 

12. Peumans M, Kanumilli P, De Munck J, van Landuyt K, Lambrechts P, van 

Meerbeek B. Clinical effectiveness of contemporary adhesives: A systematic 

review of current clinical trials. Dent Mater 2005;21:864-881. 

13. Siegel S. Nonparametric Statistics. New York: McGraw-Hill, 1956. 

14. Tay FR, Pashley DH. Water-treeing – a potential mechanism for degradation 

of dentin adhesives. Am J Dent 2003;16:6-12. 

15. Tay FR, Pashley DH, Yiu CKY, Sanares AME, Wei SHY. Factors contributing to 

the incompatibility between simplified-step adhesives and self-cured or dualcured 

composites. Part I. Single-step self-etch adhesive. J Adhes Dent 

2003;5:27-40. 

16. Türkün LS. The clinical performance of one- and two-step self-etching adhesive 

systems at one year. J Am Dent Assoc 2005;136:656-664. 

Clinical relevance: The adhesive showed a good clinical 

performance during the 2 year follow-up in noncarious cervical 

lesions. 


Sarrett 


Shear Bond Strength and Physicochemical Interactions 

of XP Bond 

Mark A. Latta a 

Purpose: The purpose of this study was to evaluate the shear bond strength of composite to dentin and enamel using 

the new etch-and-rinse adhesive XP Bond compared to other adhesives (Optibond Solo Plus, Apder ScotchBond 1 XT, 

Syntac Classic). 

Materials and Methods: Shear bond strength (MPa) was measured by shearing a resin cylinder 4.5 mm in diameter 

from prepared buccal surfaces of human third molars using an Instron Testing Machine equipped with a chiselshaped 

rod. In addition, micro-Raman spectroscopy was performed to determine if there was a chemical interaction 

between the resin adhesive and dentin and enamel. 

Results: Significant differences were observed among the dentin and enamel values generated with the adhesives 

tested. XP Bond generated statistically similar values to Optibond Solo Plus and Apder ScotchBond 1 XT to both 

enamel and dentin. Syntac Classic generated significantly lower values to both enamel and dentin. 

Conclusion: Micro-Raman spectroscopy showed a complete infiltration of resin into the demineralized dentin zone. In 

addition, it strongly suggested a chemical interaction with XP Bond and components of dentin. It is hypothesized that 

this interaction is due to the formation of calcium phosphate complexes derived from mineral apatite in the dentin 

and phosphate esters in the adhesive. 

Keywords: adhesion, bonding, chemical analysis, Raman spectroscopy. 


In spite of significant improvements in dental adhesives in 

the last decade, achieving a durable bond and seal of 

resin based restorative materials still remains a challenge. 

The primary mechanism for bonding to dentin with etch-andrinse 

adhesives is via the removal of the dentin smear layer 

and surface mineral followed by infiltration and entanglement 

of resin monomers into the exposed collagen matrix in 

the demineralized zone. 2 This resultant mixture of resin, collagen, 

and mineral is termed the hybrid zone. 4 The exposed 

collagen fibrils are suspended in water, creating space for 

a Associate Dean for Research, Professor of General Dentistry, Creighton University 

School of Dentistry, Omaha NE, USA. 



Reprint requests: Prof. Mark A. Latta, D.M.D., M.S., Associate Dean for Research, 

Professor of General Dentistry, Creighton University School of Dentistry, 

2500 California Plaza, Omaha NE 68178, USA. Tel: +1-402-280-5044, Fax: +1- 

402-280-5004. e-mail: mlatta@creighton.edu 

the penetration of the resin monomers. Drying collagen results 

in its collapse and may prevent full infiltration of the adhesive 

resin. 3 Clinically, it is difficult to create the optimal 

dentin moisture for bonding. However, failure to do so may 

lead to postoperative sensitivity, bond failure, leakage, and 

ultimately early failure of the restoration. 

There are numerous in-vitro testing methods to evaluate 

the properties of resin adhesives. While bond strength testing 

does not definitively predict clinical behavior, comparison 

of new systems with adhesives of known clinical performance 

can yield valuable information. 1,5,9 Microscopically, 

the interfacial interaction between adhesive and tooth structure 

is typically investigated with scanning electron microscopy 

and transmission electron microscopy. However, 

there is only limited chemical structural investigation of the 

resin/tooth interface. The minimal thickness of the 

tooth/adhesive interface requires an analytical technique 

with very high resolution. Micro-Raman spectroscopy has 

been shown to be a very promising technique for investigating 

the adhesive bond with tooth structure. 7,8,10,11 It has numerous 

advantages, including the ability to analyze speci- 


Latta 

Table 1 Mean shear bond strength (SBS) for each group (in MPa) 

Bonding Agent Mean SBS to dentin (MPa) Mean SBS to enamel (MPa) 

Optibond Solo plus 26.5 ± 2.9 28.3 ± 4.8 

XP Bond 25.8 ± 2.6 28.3 ± 4.7 

Adper Scotchbond 1 XT 24.2 ± 3.4 26.5 ± 4.9 

Syntac Classic (15-s etch) 13.2 ± 3.7* 21.6 ± 5.8* 

* Significantly different compared to the other groups (p < 0.05) 

mens in air or water, at room temperature and pressure, and 

without destroying the specimen. 

A new etch-and-rinse adhesive called XP Bond has been 

developed that has several unique compositional components. 

It is hypothesized that these components will allow 

the adhesive formula to be less sensitive to residual dentin 

moisture and allow full resin penetration under a wide range 

of dentin conditions. Second, this adhesive contains phosphate 

esters that may chemically interact with the mineral 

apatite component of dentin and enamel. The purpose of 

this study was to evaluate the shear bond strength of composite 

to dentin and enamel using this new adhesive system. 

In addition, micro-Raman spectroscopy was performed to 

determine if there was a chemical interaction between the 

resin adhesive and dentin and enamel. 


Shear Bond Strength 

Flat bonding sites were prepared on the buccal surfaces of 

96 extracted human teeth by grinding the teeth on a watercooled 

abrasive wheel (Ecomet III Grinder, Lake Bluff, IL, 

USA) to a 600-grit surface exposing dentin on 48 specimens 

and enamel on 48 specimens. Twelve specimens each for 

enamel and dentin for each adhesive were prepared. The adhesives 

and conditions of use were: 

• Group 1: XP Bond (lot 0503004020) cured for 10 s with 

the SmartLite LED curing light. 

• Group 2: Optibond Solo Plus (lot 437041) cured for 10 s 

with the SmartLite LED curing light. 

• Group 3: Adper Scotchbond 1 XT (lot 230270) for 10 s 

with the SmartLite LED curing light. 

• Group 4: Syntac Classic (lot G06551) using phosphoric 

acid etch 15 s and cured for 10 s with the SmartLite LED 

curing light. 

DeTrey tooth conditioner (Dentsply Detrey; Konstanz, Germany; 

lot 0403000687) was used to condition all surfaces 

prior to placement of the adhesive. After the application of 

the adhesive system, cylinders of composite resin (Spectrum 

TPH Shade A2, lot 0411002236; Dentsply DeTrey; Konstanz, 

Germany) were bonded to each dentin and enamel 

bonding site. A gelatin capsule technique in which a resin 

cylinder 4.5 mm in diameter is employed as a matrix was 

used. Composite was loaded in the capsules approximately 

two-thirds full, then cured in a Triad 2000 curing unit (Trubyte 

Division, DENTSPLY International; York, PA, USA) for 1 min. 

Additional composite was added to slightly overfill the capsules. 

The capsules were firmly seated against the bonding 

sites and excess resin removed with a dental explorer. The 

resin was visible-light cured with three 20-s curing sequences, 

each from opposite sides of the capsule at an angle 

of 45 degrees to the tooth surface. 

The specimens were stored in distilled water at 37°C for 

24 h. Twelve specimens for each adhesive/tooth structure 

combination were thermocycled between water baths of 5°C 

and 55°C for 6000 cycles (dwell time 20 s). The specimens 

were mounted in acrylic and loaded to failure in an Instron 

Testing Machine (Model 1123, Instron; Canton, MA, USA) 

equipped with a chisel-shaped rod. Each bonded cylinder 

was placed under continuous loading at 5 mm per min until 

fracture occurred. Shear bond strength was calculated in 

MPa. 

Raman Spectroscopy 

Extracted third molars were prepared by grinding enamel 

and dentin to a 600-grit surface. The experimental adhesive 

was applied and composite resin placed over the adhesive 

film. After water storage, the teeth were sectioned to expose 

the tooth/adhesive interface and polished to 4000 grit with 

silicon carbide paper. Specimens were placed on an X-Y 

scanning stage in a Jasco 3100 laser Raman Spectrometer 

(Jasco; Tokyo, Japan). The excitation was derived from a 

785-nm source at an output level of 35 mW and focused 

through an X100 near-IR lens to ~ 1 μm beam diameter. 

Wavenumber calibration was determined by comparison of 

spectra from pure silicon (520 cm -1 ). 

RESULTS AND DISCUSSION 

Shear Bond Strength 

The mean shear bond strength (in MPa) for each group is displayed 

in Table 1. A one-way ANOVA was done for the dentin 

and enamel groups. The level of significance for dentin was 

p < 0.0001, and for enamel p = 0.0168. A post-hoc LSD test 

was done for pair-wise comparison. The group marked by an 

asterisk was statistically different compared to the other 

groups (p < 0.05). 


Latta 

Fig 1 Representative spectra of dentin (left) and dentin impregnated with XP Bond (right). Circle represents peak shift and broadening in 

the 1100 to 1170 cm -1 range is suggestive of calcium-phosphate ester complex formation. 

Fig 2 Representative spectrum of XP Bond showing major functional 

groups. Plot of peak intensity vs wavenumber cm -1 . 

Fig 3 Peak intensity for characteristic marker peaks for dentin, 

mineral and resin are plotted across the dentin/adhesive interface. 

The resin peak at 1720 cm -1 fully penetrates to the bottom 

of the demineralized zone. In addition, the maximum strength of 

the 1146 cm -1 peak is offset from the resin, indicating an interaction 

with components in the dentin layer. 

Raman Spectroscopy 

A representative spectrum of XP Bond is shown in Fig 1. Representative 

Raman spectra of human dentin and resin impregnated 

dentin with XP Bond are shown in Fig 2. The most 

intense band occurs at 960 cm -1 and is associated with the 

P-O stretch of the phosphate in the mineral apatite. Also observed 

are bands at 1245 cm -1 (amide III) and 1667 cm -1 

(amide I) associated with collagen. The mixture shown on the 

right clearly shows the apatite and amide I peaks mixed with 

features only associated with the adhesive. The peak shift 

and broadening in the 1100 to 1170 cm -1 area is not seen 

in the pure dentin or XP Bond spectrum, and is associated 

with the formation of calcium/phosphate ester complexes in 

the hybrid layer. 6 

The relative peak intensities of the mineral apatite (960 

cm -1 ), resin carbonyl (1720 cm -1 ), collagen (1670 cm -1 ), and 

phosphate complex (centered at 1146 cm -1 ) were plotted 

across the dentin interface and are shown graphically in 

Fig 3. The strength of the phosphate complex intensity in the 

intermediate hybrid layer is strongly suggestive of a chemical 

interaction between components in the resin adhesive 

and the dentin. In addition, the resin is fully penetrated to 

the depth of the zone of demineralization. 

CONCLUSION 

Significant differences in shear bond strength were observed 

among the dentin and enamel values generated with 

the adhesives tested. XP Bond generated statistically similar 

values to Optibond Solo Plus and Apder ScotchBond 1 XT 

to both enamel and dentin. Syntac Classic generated significantly 

lower values to both enamel and dentin. 

Micro-Raman spectroscopy showed a complete infiltration 

of resin into the demineralized dentin zone. In addition, 

it strongly suggested a chemical interaction with XP Bond 


Latta 

and components of dentin. It is hypothesized that this interaction 

is the formation of calcium phosphate complexes derived 

from mineral apatite in the dentin and phosphate esters 

in the adhesive. 


This research was partly sponsored by Dentsply DeTrey, Konstanz, 

Germany. 

6. Penel G, Leroy N, Rey C, Lemaitre J, Van Landuyt P, Ghanty N. Qualitative 

and quantitative investigation of calcium phosphate of biological interest 

by Raman micro-spectrometry. Recent Res Develop Appl Spectroscopy 

1999;2:137-146. 

7. Sato M, Miyazaki M. Comparison of depth of dentin etching and resin infiltration 

with single-step adhesive systems. J Dent 2005;22:475-484. 

8. Spencer P, Wang Y, Walker MP, Wieliczka DM, Swafford JR. Interfacial 

chemistry of the dentin/adhesive bond. J Dent Res 2000;79:1458-1463. 

9. Shaddy RS, Latta MA, Goren M. The effect of salivary contamination on adhesive 

shear bond strength. J Pract Hygiene 2003;12:27-28. 

10. Wang Y, Spencer P. Hybridization efficiency of the adhesive dentin interface 

with wet bonding. J Dent Res 2003;82:141-145. 

11. Wang Y, Spencer P. Physicochemical interactions at the interface between 

self-etch adhesive systems and dentine. J Dent 2004;32:567-579. 

REFERENCES 

1. Barkmeier WW, Hamesfahr PD, Latta MA. Bond strength of composite to 

enamel and dentin using Prime and Bond 2.1. Oper Dent 1999;24:51-56. 

2. Eick JD, Gwinnet AJ, Pashley DH, Robinson SJ. Current concepts in adhesion 

to dentin. Crit Rev Oral Biol Med 1997;8:306-335. 

3. Gwinnett AJ. Quantitative contribution of resin infiltration/hybridization to 

dentin bonding. Am J Dent 1993;6:7-9. 

4. Nakabayashi N, Kijima K, Masuhara E. The promotion of adhesion by the 

infiltration of monomers into tooth substrates. J Biomed Mater Res 

1982;16:265-273. 

5. Naughton WT, Latta MA. Bond strength of composite to dentin using selfetching 

adhesive systems. Quintessence Int 2005;36:41-44. 

Clinical relevance: The laboratory bond values for a 

newly developed etch and rinse adhesive system would 

suggest exellent clinical performance. The discovery of 

chemical interaction between the adhesive and the mineral 

component of tooth structure may help explain the 

high bond strengths and also might predict the generation 

of a stable long term bond interface clinically. 


Microshear Fatigue Testing of Tooth/Adhesive 

Interfaces 

Marc Braem a 

Purpose: The objective of the present study was to determine the fatigue resistance of several contemporary dentin 

adhesives as well as a resin-modified glass-ionomer cement. 

Materials and Methods: Cyclic loading of the adhesive interface was achieved by a microshear fatigue setup following 

a staircase approach, where the stress level at which 50% of the specimens fail after 10 4 cycles was calculated 

as the median microshear fatigue resistance (μSFR). 

Results: For all products tested, the μSFR was lower than the microshear strength. A wide spread in μSFR was observed, 

ranging from 24% to 76% of the quasi-static microshear strength, irrespective of the type of adhesive used. 

Conclusion: The results of this study show that the microshear test setup is a discriminative and reproducible way of 

testing tooth/adhesive interfaces, even at relatively low stresses. The results clearly indicate that such interfaces are 

vulnerable to progressive damage by cyclic loads. Further, at present there is not one bonding approach, whether 

“total etch” or “self-etching”, that consistently yields higher fatigue resistance: the product factor seems to be of primary 

importance. 

Keywords: fatigue, dental adhesive, dynamic testing. 


The success of bonding restorative materials to tooth tissue 

is generally expressed as a statically or quasi-statically 

determined strength value. Under clinical circumstances, 

however, tooth-restorative bonds are subjected to 

cyclic loads that could well induce failure at stress levels significantly 

lower than the ultimate bond strength, a phenomenon 

defined as fatigue. 1 In addition, under fatigue conditions, 

the influence of imperfections in the adhesive interface 

is more clearly revealed. 7 At present, research on 

dentin bonding is, among other things, focused on reducing 

the number of application steps in the bonding procedure, 

thereby assuming a reduction in the risk of defects. In vitro 

a Professor, Head of Lab Dental Materials, University of Antwerpen, Antwerpen, 

Belgium. 



Reprint requests: Dr. Marc Braem, Lab Dental Materials, Groenenborgerlaan 

171, B-2020 Antwerpen, Belgium. Tel: +32-3-265-32-66, Fax: +32-3-265- 

36.35. e-mail: marc.braem@ua.ac.be 

fatigue testing of these interfaces could therefore better allow 

studying these effects. 

Hence, the objective of this study was to determine the 

fatigue resistance of several contemporary dental adhesives 

and a resin-modified glass-ionomer cement bonded to 

dentin, using a custom-built microshear fatigue testing device. 


Materials 

The materials used are shown in Table 1. All tests were performed 

prior to the expiration date mentioned in the table. 

The composite restorative used with dentin bonding was 

Clearfil AP-X (Universal Shade A3, Lot 1043 BA; Kuraray, 

Japan). All applications were performed as per manufacturer’s 

instructions. 

Dentin Specimen Preparation 

Dentin collected after extraction of human third molars was 

used. The teeth were stored immediately in chloramine 0.5% 


Braem 

Table 1 Materials used 

Brand name Manufacturer Type Primer Adhesive Light-curing resin 

Batch Exp Date Batch Exp Date Batch Exp Date 

Fuji II LC Capsules GC Europe glass-ionomer cement 301241 2005-01 

Syntac Vivadent 3-step etch and rinse G01297 2006-05 G04548 2006-08 G03430 2009-01 

Optibond FL Kerr 3-step etch and rinse 403204 2006-01 402145 2005-06 

Optibond Solo Plus Kerr 2-step etch and rinse 3-1325 2005-11 

Prime & Bond NT Dentsply DeTrey 2-step etch and rinse 0503000835 2008-02 

XP Bond Dentsply DeTrey 2-step etch and rinse 503004020 2005-11 

Adper ScotchBond 1 XT 3M ESPE 3-step etch and rinse 4AG 20040424 2007-02 

Clearfil SE Bond Kuraray 2-step SE 41460 2008-02 

Clearfil Protect Bond Kuraray 2-step SE 61112 2005-12 

Xeno III Dentsply DeTrey 1-step SE 2 components 0512000738 2007-11 

Adper Prompt-L-Pop 3M ESPE 1 step SE 2 components 175425 2005-09 

G-Bond GC Europe 1 step SE 1 component 0406161 2006-06 

iBond Heraeus-Kulzer 1 step SE 1 component 010082 2008-08 

at 5°C prior to cutting, which was done within 30 days after 

extraction. 

After removal of the roots and pulp tissue, the teeth were 

glued on a cubic clamp and a first cut (Microslice 2, Metals 

Research; Cambridge, UK) was made parallel to the occlusal 

surface to remove the occlusal enamel. Next, the clamp was 

rotated 90 degrees and a first series of parallel cuts 3 mm 

apart was made perpendicular to the surface. The clamp 

was then again rotated 90 degrees and a new series of cuts 

was made in an identical way. As a result, cubic samples are 

created that are broken off the remains of the tooth in order 

to make sure that perpendicularly cut tubules will be used 

in the test. 

The dentin cube was then positioned in the center of the 

base of the test jig with the test surface against a Plexiglas 

plate (Fig 1), immobilized by slight pressure. A light-curing 

glass-ionomer cement (Fuji II LC capsules, GC Europe; Haasrode, 

Belgium) was mixed for 10 s followed by 3 s in a RotoMix 

device (3M ESPE; Seefeld, Germany), applied without 

prior conditioning of the dentin, and light cured for 20 s each 

at the bottom and top surfaces using a QTH light source 

(Luxor, ICI; Manchester, UK) with an output of at least 520 

mW/cm 2 . Output was checked with a radiometer (Optilux 

Model 100, SDS Kerr; Danury, CT, USA). 

The dentin test surface was prepared using a small piece 

of 600-grit grinding paper, cleaned with compressed air and 

water, and thereafter visually inspected under a light microscope. 

The test surface was then treated according to the 

manufacturer’s instructions for the respective materials. 

When separate acid etching was required, a phosphoric acid 

gel was used (Scotchbond etching gel, 3M ESPE), except 

when a proprietary etchant is included with the adhesive, as 

is the case for Prime & Bond NT. Polyacrylic acid (GC Conditioner, 

GC Europe) was used in case of the resin-modified 

glass-ionomer cement. 

Once the final adhesive layer was finished for the dentin 

bonding, or the dentin was conditioned prior to the application 

of the resin-modified glass-ionomer cement, a perforated 

(diameter 1 mm) Mylar strip (0.05 mm thick) was accurately 

centered on top of the prepared sample and the upper 

part of the test jig was fixed (Fig 2). A first portion of the 

restorative was applied without touching the cavity walls and 

light cured. Next the remainder of the cavity was filled and 

cured incrementally. 

The test jig was then transferred to the fatigue machine 

and the screws removed (Fig 3). This method prevents the 

adhesive interface from being unintentionally touched or 

loaded by any means prior to testing. 

Fatigue Testing 

The present method is a modification of a previously described 

setup. 2 All testing was carried out at 35°C under 

load-controlled conditions, at a test frequency of 2 Hz. 

First, the quasi-static microshear strength (τ) was determined 

by measuring the maximal force at failure divided by 

the bonding surface area, which was measured under a light 

microscope prior to testing. 

During the fatigue test, the specimens were subjected to 

cyclic loading. Tests were conducted sequentially, with the 

initial stress set at about 50% of the microshear strength of 


Braem 

Fig 1 Positioning of the dentin sample with the surface to be 

tested oriented downwards on a Plexiglas plate. 

Fig 2 Top view of the test jig after preparation of the bond and 

placement of the perforated Mylar strip. The upper part of the jig 

is fixed prior to the application of the restorative material. 

the adhesive maximum and stressed until failure or 10 4 cycles. 

The applied stress in each succeeding test was increased 

or decreased by a fixed increment of stress, according 

to whether the previous test resulted in failure or no 

failure, also described as a staircase approach. 6 This fixed 

increment is based on pilot testing and fixed at 8% of the microshear 

strength. 

The results of the fatigue test were analyzed using logistic 

regression 4 to determine the load at which 50% of the 

specimens fail, further referred to as the “median microshear 

fatigue resistance” or μSFR. To compare the fatigue 

data obtained from the different experimental groups, a multiple 

logistic regression analysis was conducted (Statistica 

6.0, StatSoft; Tulsa, OK, USA). 

RESULTS 

The microshear strength and the μSFR for each material are 

given in Table 2. The μSFR was about 43% lower than the respective 

microshear strength value (Table 2), ranging from 

24% in the case of Optibond Solo Plus and iBond, up to 76% 

for Clearfil Protect Bond. 

Comparing the slope β 1 obtained from the logistic regression 

(Table 2), a very steep curve can be seen for Xeno III 

(β 1 = 6.5079) and Adper Prompt-L-Pop (β 1 = 5.8161), being 

almost 10 times steeper than that of the other resin bonding 

agents. In Xeno III, failures were noted after 145, 915, 196, 

565, 645, 1465 and 460 cycles and after 245, 1625, 150, 

1080, 550, 3595 and 270 cycles for Adper Prompt-L-Pop. 

The same can be said, although to a lesser degree, of Fuji II 

LC (β 1 = 1.1195) with failures at 75, 30, 65, 185, 55, 6750, 

40, 565, 7540, 50, and 80 cycles. G-Bond on the other hand 

shows a rather flat curve with β 1 = 0.1652, with failures noted 

at 65, 130, 135, 4430, 9475, 260, 55, and 155 cycles. 

Using the results from the logistic regression, the 25% 

Fig 3 Placement of the test jig in the fatigue machine. The jig is 

fixed using compressed air (1). The piezo-electric force transducers 

(2) record the applied loads. 

and 75% quartiles can be calculated, giving an indication of 

the range of the results around the μSFR (Table 2). Comparing 

the different adhesives using multiple logistic regression, 

the bond strength in MPa (p < 0.0001) as well as 

the adhesive (p = 0.0003) contribute significantly to the 

model. 

DISCUSSION 

The lack of fatigue data in the dental literature on adhesive 

interfaces is profound. Only some data are available today, 

4,5,7,10,12,13 in spite of the necessity to complete the quasi-static 

bond strength tests with clinically relevant dynamic 

fatigue data. A prerequisite is that the setup is of clinical rel- 


Braem 

Table 2 Results for the microshear strength (τ, MPa) and μSFR (MPa) 

Brand name μ-shear ± SD μSFR 25% 75% β0 1 β1 1 p-value 2 τ/μSFR 

strength quartile quartile (%) 

Fuji II LC Caps 10.1 ± 3.1 4.1 3.1 5.1 -4.5580 1.1195 0.0000 41 

Syntac 55.5 ± 5.1 30.4 28.4 32.4 -16.6834 0.5492 0.0000 55 

Optibond FL 56.9 ± 3.2 17.2 13.4 21.0 -4.9682 0.2893 0.1056 30 

Optibond Solo Plus 49.2 ± 10.5 11.9 9.7 14.1 -6.1994 0.5188 0.0001 24 

Prime & Bond NT 47.0 ± 2.7 18.3 13.9 22.7 -4.5571 0.2491 0.3987 39 

XP Bond 56.4 ± 2.0 30.3 26.7 33.8 -9.3190 0.3081 0.0000 52 

Adper ScotchBond 1 XT 51.7 ± 4.8 17.9 15.7 20.1 -8.7526 0.4895 0.0585 35 

Clearfil SE Bond 35.0 ± 8.4 20.7 16.4 24.9 -5.3315 0.2577 0.5672 65 

Clearfil Protect Bond 42.8 ± 12.3 32.6 28.9 36.3 -9.7454 0.2991 0.0000 76 

Xeno III 46.2 ± 3.5 25.2 25.1 25.4 -175.7207 6.9613 0.0073 55 

Adper Prompt-L-Pop 53.5 ± 10.7 22.7 22.5 22.9 -132.0255 5.1610 0.0585 42 

G-Bond 54.9 ± 3.7 15.3 8.5 22.1 -2.4908 0.1625 0.0318 28 

iBond 51.0 ± 8.3 12.3 8.7 15.9 -3.7347 0.3042 0.0003 24 

1) β0 and β1 are parameters of the logistic regression function, determining the probability of failure in terms of stress applied to the interface (S): Y = exp(β0 + β1 •S) / (1 + exp(β0 + β1 •S)) 

2) p-value of estimate of the multiple logistic regression 

evance. Assuming 3 periods of 15 min of chewing per day 

at a chewing rate of 1 Hz, the number of chews is 2700 per 

day. 14 This amounts to roughly 10 6 times per year. At this frequency, 

a fatigue test on 1 sample takes about 12 days to 

accomplish 10 6 cycles. Increasing the rate to 2 Hz will offer 

a time-saving approach well within the frequency dependency 

range of the tested visco-elastic materials. Furthermore, 

if the noncontact events are eliminated from the 

chewing cycles, it can be calculated that 10 4 cycles represents 

about 1.2 months of continuous real-life contact. This 

approach is justified, since restorations tend to fail either 

early, before 10 4 cycles, or very late, after 10 5 cycles. 9 Moreover, 

a test run on a sample that does not fail now takes 

about 1.5 h to complete, as opposed to about 1 week for 

10 6 cycles. 

A common standard in the analysis of fatigue data is the 

value at which 50% of the specimens fail after a pre-set number 

of cycles. 2,4,5 However, in the present type of fatigue testing, 

considerable errors can be made as to the determination 

of the so-called pre-set stress levels due to geometry errors. 4 

Therefore, the probability of failure at each applied stress level 

was approximated by logistic regression where the μSFR 

represents the value at which 50% of the specimens fail. Calculating 

the 25% and 75% quartiles further illustrates the 

distribution of the obtained data (Table 2). It can be seen 

from these data that the products with the steepest slopes 

(β 1 ) show the lowest distribution around the μSFR. 

Some of the adhesives therefore show a so-called type 2 

fatigue behavior 10 and appear to have a rather well-defined 

fatigue stress level or threshold above which they fail rapidly 

and below which they will survive (Xeno III, Adper Prompt- 

L-Pop, Fuji II LC). In other products, such as G-Bond, the opposite 

behavior is found and a wide spread of data around 

the μSFR can be noted. Most of the materials show a mixed 

type of behavior, indicating that imperfections and defects 

probably determine the actual lifespan of the adhesive 

bond. Fractographic analysis needs to be carried out to test 

this hypothesis. 

The main advantage of the present method is that with 

the same setup, both shear strength and fatigue resistance 

can be measured and compared. It is also advantageous 

that the method requires no processing of the sample once 

the interface has been formed, thereby avoiding operator-induced 

defects. The results show that the μSFRs are consistently 

lower than the respective microshear strength for the 

same adhesive (Table 2). This is not surprising, since it is 

known that internal interfacial defects and imperfections 

shorten the lifespan of a joint under cyclic fatigue. Hence, 

fatigue data generally vary substantially more than static 

bond strengths. 8 The present results, however, show in 

some cases that the variation in the fatigue data is lower 

than that present in the quasi-static data, thereby emphasizing 

the need for nontraumatic sample preparation. 

It is beyond the scope of the present article to discuss in 

full the possible mechanism of each individual adhesive related 

to the measured μSFR. The present results emphasize 

that within each type of adhesive, products exist that show 

a high fatigue resistance. Furthermore, some few-step adhesives 

perform better than other multi-step ones, while for 

others it is just the opposite. Thus, not only the reduction in 


Braem 

the number of steps but also the degree of difficulty of the 

step appears to be of primary importance. 

The present results indicate that the fatigue behavior of 

each individual adhesive must be carefully studied, since 

within each group results can be found that outperform 

and/or are similar to results obtained by particular adhesives 

in other groups. This indicates that, in general, the different 

types of bonding approaches converge to adequate 

results. In this context, the result for the glass-ionomer cement 

is surprising: both the microshear bond strength and 

the μSFR are among the lowest measured in this study. This 

can be explained by a mismatch in the mechanical properties 

of the glass-ionomer matrix and the glass particles, 

causing large stresses to accumulate at their interface. 11 

However, the clinical performance of these materials under 

the right indications is still remarkably good, thus supporting 

the hypothesis that “self-healing” or “repair” might be 

possible in glass-ionomer cements, 3 although such “healing” 

may rather be retardation in crack growth or a crack 

growth toughening mechanism due to the plasticizing effect 

of the resinous component. 

CONCLUSION 

Tooth/adhesive interfaces suffer from the progressive damage 

induced by subcritical cyclic loads. The differing approaches 

to achieving tooth-resin bonding are not consistently 

reflected in differences in fatigue resistance. 


The author thanks the manufacturers for the generous donation of materials. 

Thanks also to Dr. Jan De Munck, Leuven BIOMAT Research 

Cluster K.U. Leuven, Belgium, the statistical analysis could be performed. 

Finally, the supporting efforts and constructive criticism of Mr. 

Geert Keteleer, Lab Dental Materials – Universiteit Antwerpen, are 

greatly acknowledged. 

This research was partly sponsored by Dentsply DeTrey, Konstanz, 

Germany. 

REFERENCES 

1. Baran GR, Boberick KG, McCool JI. Fatigue of restorative materials. Crit 

Rev Oral Biol Med 2001;12:350-360. 

2. Braem M, Davidson CL, Lambrechts P, Vanherle G. In vitro flexural fatigue 

limits of dental composites. J Biomed Mater Res 1994;28:1397-1402. 

3. Davidson CL. Glassionomer bases under posterior composites. J Esthet 

Dent 1994;6:223-226. 

4. De Munck J, Braem M, Wevers M, Yoshida Y, Inoue S, Suzuki K, Lambrechts 

P, Van Meerbeek B. Micro-rotary fatigue of tooth-biomaterial interfaces. 

Biomater 2005;26:1145-1153. 

5. Dewji HR, Drummond JL, FadaviS, Punwani I. Bond strength of bis-GMA 

and glass ionomer pit and fissure sealants using cyclic fatigue. Eur J Oral 

Sci 1998;6:594-599. 

6. Draughn RA. Compressive fatigue limits of composite restorative materials. 

J Dent Res 1979;58:1093-1096. 

7. Givan DA, Fitchie JG, Anderson L, Zardiackas LD. Tensile fatigue of 4-META 

cement bonding three base metal alloys to enamel and comparison to 

other resin cements. J Prosthet Dent 1995;73:377-385. 

8. Hawbolt EB, MacEntee MI. Effects of fatigue on a soldered base metal 

alloy. J Dent Res 1983;62:1226-1228. 

9. Huysmans MCDNJM, Van der Varst PGT, Schäfer R, Peters MCRB, Plasschaert 

AJM, Soltész U. Fatigue behavior of direct post-and-core-restored 

premolars. J Dent Res 1992;71:1145-1150. 

10. McCabe JF, Carrick TE, Chadwick RG, Walls AWG. Alternative approaches 

to evaluating the fatigue characteristics of materials. Dent Mater 

1990;6:24-28. 

11. Nakajima H, Watkins JH, Arita K, Hanaoka K, Okabe T. Mechanical properties 

of glass ionomers under static and dynamic loading. Dent Mater 

1996;12:30-37. 

12. Nikaido T, Kunzelmann K-H, Chen H, Ogata M, Harada A, Yamaguchi Y, Cox 

CF, Hickel R, Tagami J. Evaluation of thermal cycling and mechanical loading 

on bond strength of a self-etching primer system to dentin. Dent Mater 

2002;18:269-275. 

13. Ruse ND, Shew R, Feduik D. In vitro fatigue testing of a dental bonding system 

on enamel. J Biomed Mater Res 1995;29:411-415. 

14. Wiskott HWA, Nicholls JI, Belser UC. Fatigue resistance of soldered joints: 

A methodological study. Dent Mater 1994;10:215-220. 

Clinical relevance: Repetitive shear loading off freshly 

placed adhesive fillings will impose subcritical loads 

that could finally induce damage and/or loss of the adhesion. 

The study of such behavior is therefore of utmost 

importance in order to gain knowledge on this 

type of failure 


Sarrett 


Microleakage of Class V Composite Restorations Placed 

with Etch-and-Rinse and Self-etching Adhesives Before 

and After Thermocycling 

Juan Ignacio Rosales-Leal a 

Purpose: To evaluate the sealing ability of etch-and-rinse and self-etching adhesives in Class V cavities before and 

after thermocycling in vitro. 

Materials and Methods: Etch-and-rinse adhesives (Prime & Bond NT [P&B], XP Bond [XPB], ScotchBond 1 XT [SBX], 

Syntac [SYN]) and self-etching adhesives (Xeno III [XNO], i-Bond [IBO], Clearfil SE Bond [CLF]) were used. A microleakage 

test was performed to evaluate marginal sealing. Seventy molars were divided into seven groups according to the 

adhesive used. Class V cavities were restored and each group was divided into two subgroups. One group was water 

immersed for 24 h and the other was thermocycled. Then, specimens were immersed in fuchsin and sectioned. Microleakage 

and dentin permeability were recorded on occlusal and gingival walls and data were statistically analyzed. 

Results: Etch-and-rinse adhesives provided perfect occlusal sealing. Self-etching adhesives obtained slight occlusal 

leakage. In the gingival wall, XNO and CLF showed the lowest leakage, followed by XPB and SBX, then P&B. SYN and 

IBO exhibited the highest leakage. All SE adhesives and XPB provided sealed dentinal tubules. Thermocycling did not 

affect the occlusal sealing but reduced the gingival sealing when P&B, SYN, XNO, CLF, and IBO were used. 

Conclusion: In enamel, marginal leakage was prevented when phosphoric acid was used. Self-etching adhesives promoted 

slight occlusal leakage. The gingival sealing was poorer than the occlusal sealing. XNO, CLF followed by XPB 

obtained the best gingival sealing. Thermocycling did not affect the occlusal bonding but reduced the gingival sealing, 

except when XPB and SBX were used. 

Keywords: adhesives, Class V sealing, thermocycling, in vitro. 


Sealing of a cavity is one of the most important requirements 

for the durability of a composite restoration. 13 Microleakage 

of a restoration may be the starting point of secondary 

caries and the treatment failure. 11 The bond needs 

to be hermetic but also durable over time. 3,21 

In vitro microleakage tests offer very useful data about 

the sealing behavior of adhesives. A microleakage test provides 

information about the sealing of the interface and the 

dentin tubule sealing (dentin permeability). 1,16 Results are 

close to clinical reality because extracted human teeth and 

clinical protocols are used. 7,11 

Two different classes of adhesives are currently used. 

Etch-and-rinse adhesives require a separate acid-etching 

step prior to the adhesive infiltration that promotes an aggressive 

substrate treatment. 15 Self-etching adhesives etch 

and infiltrate at the same time, but their acidity is less than 

that of phosphoric acid, resulting in less etching depth. 19 

More information is necessary about the sealing ability of 

current adhesives (etch-and-rinse vs self-etching) and the effect 

of aging on the durability of the sealing. The purpose of 

this work was to evaluate the in vitro sealing ability of etchand-rinse 

and self-etching adhesives in Class V cavities before 

and after thermocycling. 

a Assistant Professor, Department of Stomatology (Dental Materials), University 

of Granada, Granada, Spain. 



Reprint requests: Dr. Juan Ignacio Rosales-Leal, Camino de Ronda, 57-2ºB, 

18004 Granada, Spain. Tel: + 34-653-32-03-84, Fax: +34-958-240-908. 

e-mail: irosales@ugr.es 


The adhesives used are described in Table 1. Seventy third 

molars were divided into 7 groups as a function of the adhesive 

used (Table 1). In each specimen, two Class V Cavities 

(3 x 2 x 2 mm [depth] with a 1-mm 45-degree enamel 


Rosales-Leal 

Table 1 Materials tested 

Adhesive 

Manufacturer 

Components 

Directions for use 

Prime & Bond NT 

lot: 0503000835 

(P&B) 

Dentsply DeTrey; 

Konstanz, Germany 

Conditioner: DeTrey Conditioner (36% 

phosphoric acid) 

Adhesive: (resin, di- and trimethacrylate, 

amorphous functional, 

silica, PENTA, cetyl amine 

hydrofluoride, acetone, photoinitiators, 

stabilizers) 

Composite: Esthet·X (microhybrid) 

Etch the cavity for 15 s, wash and dry but do 

not desiccate. Apply the adhesive and wait 

for 20 s. Dry and polymerize for 10 s. Apply 

composite and polymerize for 20 s. 

XP Bond 

lot: 0503004020 

(XPB) 

Dentsply, DeTrey; 


Conditioner: DeTrey Conditioner (36% 

phosphoric acid) 

Adhesive: tertiary butanol, HEMA, 

PENTA, TCB, UDMA, TEG-DMA; 

butylated benzenediol, ethyl-4- 

dimethylaminobenzoate, camphoroquinone, 

nanofillers 

Composite: Ceram·X mono (nano 

ceramic) 

Etch the cavity for 15 s, wash and dry but do 

not desiccate. Apply adhesive and wait for 

20 s. Dry and polymerize for 10 s. Apply 

composite and polymerize for 20 s. 

Adper ScotchBond 1 XT 

lot: 177215 

(SBX) 

3M; St Paul, MN, USA 

Conditioner: etchant (37% phosphoric 

acid) 

Adhesive: HEMA 

Composite: Filtek Supreme (nano 

composite) 

Etch cavity for 15 s, wash and dry (do not 

desiccate). Apply adhesive and wait for 15 s. 

Air dry and light cure for 10 s. Place composite 

and light cure for 20 s. 

Syntac 

lot: G01297 

[primer], G04548 

[adhesive], 

G03430 [bonding] 

(SYN) 

Ivoclar Vivadent; 

Schaan, Liechtenstein 

Conditioner: Total Etch (37% 

phosphoric acid). 

Primer: polyethylene glycol dimethacrylate, 

maleic acid, ketone, water 

Adhesive: polyethylene glycol 

dimethacrylate, glutaraldehyde, water 

Bonding: bis-GMA, TEG-MA 

Composite: Tretic Evo Ceram 

(microhybrid) 

Etch cavity for 30 s, wash and dry. Apply 

primer, wait for 15 s. Air dry. Apply adhesive 

and wait 10 s. Air dry. Apply bonding and air 

dry. Light cure for 10 s Place composite and 

light cure for 20 s. 

Xeno III 

lot: 0403001320 

[A liquid], 

0403001320 

[B liquid] (XNO) 

Dentsply, DeTrey; 


Adhesive: A liquid (HEMA, water, 

ethanol, BHT, highly dispersed silicon 

dioxide). B liquid (pyro-EMA, PEM-F, 

UDMA, BHT, camphoroquinone, ethyl- 

4-dimethylaminobenzoate). 

Composite: Ceram·X mono (nano 

ceramic) 

Mix liquid A and B. Apply in the cavity and 

wait for 20 s. Dry and polymerize for 10 s. 

Apply composite and polymerize for 40 s. 

i-Bond 

lot: 010082 

(IBO) 

Heraeus Kulzer; 

Hanau, Germany 

Adhesive: acetone, water, 

methacrylate resins, glutaraldehyde 

Composite: Venus (microhybrid) 

Apply a copious amount to the cavity. Apply 

two additional coats. Wait for 30 s. Dry and 

polymerize for 20 s. Apply composite and 

polymerize for 20 s. 


lot: 00453A 

[primer]; 00623A 

[adhesive] 

(CLF) 

Kuraray; 

Okayama, Japan 

Primer: MDP, HEMA, hydrophilic 

dimethacrylate, di-camphorquinone, 

N,N-diethanol-p-toluidine, water 

Bonding: MDP, bis-GMA, HEMA, 

hydrophobic dimethacrylate, di-camphoroquinone, 

N,N-diethanol-ptoluidine, 

silanated colloidal silica 

Composite: Clearfil AP X (microhybrid) 

Apply primer; wait for 20 s. Dry with mild air 

flow. Apply bond. Air flow gently. Light cure 

for 10 s, place composite and polymerize for 

40 s. 

HEMA: 2-hydroxyethylmethacrylate; PENTA: dipentaerythriol penta acrylate monophosphate; TCB: carboxylic acid modified dimethacrylate; TEG-DMA: triethyleneglycol 

dimethacrylate; pyro-EMA: phosphoric acid modified methacrylate; PEM-F: monofluorophosphazene-modified methacrylate; MDP: 10- 

methacryloyloxydecyl dihydrogen phosphate; UDMA: urethane dimethacrylate; bis-GMA: bis-phenol A diglycidyl methacrylate. 


Rosales-Leal 

Fig 1 Percentage of cases with each 

microlekage grade on the occlusal wall 

(O) and on the gingival wall (G) after 

24-h water immersion (24 h) and 

4000 cycles of thermocycling (4000 

c). Columns with the same letter are 

statistically similar (p > 0.05). 

bevel) were prepared with diamond-coated #330 burs at 

high speed under water cooling. Cavities were filled following 

manufacturer’s directions for use. The filling material 

was placed in two increments. The LED unit SmartLite PS 

(Dentsply DeTrey; Konstanz, Germany) (light output: 830 

mW/cm 2 ) was used for polymerization. The restoration was 

finished and polished with abrasive disks. Restored teeth 

were divided into two subgroups. In one group, teeth were 

kept in water at 37°C for 24 h. In the other group, teeth were 

thermocycled 4000 times between water baths at 5°C and 

55°C with a dwell time in each bath of 30 s. After sealing the 

roots with IRM (Dentsply DeTrey), the teeth were covered with 

two coats of nail varnish, leaving a 1-mm varnish-free margin 

around the restoration. Specimens were then immersed 

in a 0.5% water solution of basic fuchsin for 24 h and rinsed 

for 5 min with water. After this, specimens were embedded 

in acrylic resin, and 3 buccolingual slices of 1 mm thickness 

were obtained from each specimen (15 slices resulting in 30 

margins in dentin and enamel, per adhesive and aging condition). 

Slices were coded and randomly examined independently 

under the microscope in a blinded fashion. The 

grade of microleakage at occlusal and gingival walls was categorized 

as follows: 0: hermetic seal, no leakage; 1: mild microleakage, 

dye on no more than half of the wall; 2: moderate 

microleakage, dye on more than half of the wall but not 

including the axial wall; 3: massive microleakage, dye on the 

entire wall, including the axial wall. Data obtained represent 

the percentage of each leakage score in all the analyzed 

slices. Dentin permeability was evaluated as negative (absence 

of dye solution in dentin tissue) or positive (presence 

of dye solution in dentin tissue). Microleakage analysis was 

performed with the nonparametric Kruskal-Wallis H-test and 

Mann-Whitney U-test (p < 0.05). Fisher’s Exact test was used 

to evaluate dentin permeability (p < 0.05). 

RESULTS 

Figures 1 and 2 show the microleakage and dentin permeability 

data. The occlusal wall exhibited less leakage than the 

gingival wall. Etch-and-rinse adhesives achieved hermetic 

occlusal sealing, while self-etching adhesives showed slight 

occlusal leakage. Occlusal dentin permeability was negative 

for all the adhesives tested. Thermocycling did not affect the 

occlusal sealing. 

On the gingival wall, XNO and CLF obtained the lowest 

leakage, followed by XPB, SBX, and P&B, while SYN and IBO 

showed the highest leakage. Thermocycling did not affect 

marginal seal in dentin for XPB and SBX, with the latter 

showing more leakage after thermocycling compared to 

XPB. However, marginal seal of P&B, SYN, XNO, IBO, and CLF 

was influenced by thermocycling. Dentin permeability was 

negative for XPB, XNO, IBO and CLF. Positive dentin permeability 

was observed when P&B, SBX or SYN were used. Thermocycling 

increased the dentin positive permeability of P&B 

and SYN groups. 

DISCUSSION 

This in-vitro test provoked microleakage for all adhesives 

used. Three main factors could affect the sealing. One factor 

is the composite polymerization shrinkage that induces 

stress at the bonding interface. 8 This stress can potentially 


Rosales-Leal 

Fig 2 Percentage of cases with positive 

and negative permeability on the 

occlusal wall (O) and on the gingival 

wall (G) after 24-h water immersion 

(24 h) and 4000 cycles of thermocycling 

(4000 c). Columns with the 

same letter are statistically similar (p 

> 0.05). 

break the bond and facilitate leakage. 13,19 Another factor is 

that the substrate is a biological tissue, which makes adhesion 

difficult. 15 The third factor is the adhesive itself: the 

chemical composition plays an important role in achieving a 

strong, durable, and biologically compatible bond. 11 

Etch-and-rinse adhesives obtained hermetic sealing on 

the occlusal wall, which is surrounded by enamel. Enamel is 

mainly composed of minerals with no significant amount of 

organic compounds or water. 15 Use of phosphoric acid leads 

to pronounced etching depth. The adhesive covers a highly 

irregular mineral surface with no water, creating a hermetic 

and strong bond. 2,6,9,10,13 In contrast, self-etching adhesives 

exhibited slight leakage. In general, the pH of acidic 

primers is higher than that of phosphoric acid, resulting in a 

less pronounced etching effect. 4,21 The consequence in this 

in vitro study was a weaker bond with slight leakage. 6,8,15 

In agreement with other studies, 6,8,10,13,14 sealing was 

better along occlusal than gingival margins. The gingival wall 

is formed by dentin, which consists of minerals, organic 

compounds (mainly collagen fibers), and water. 15 In addition, 

dentin tubules cross the tissue and are full of water. After 

phosphoric acid treatment, there is a deep demineralization 

front in which the collagen network is exposed, dentin 

tubules are opened, and water content is increased. 17 Etchand-rinse 

primers have to infiltrate the exposed collagen, replace 

the water, and seal the tubules. Therefore, sealing is 

complicated, and this histological finding explains the higher 

leakage and positive permeability when etch-and-rinse adhesives 

are used. XPB was the best etch-and-rinse adhesive 

in this study, and always sealed the dentin tubules. This adhesive 

uses tertiary butanol as a solvent and provides an increase 

in resin content. After polymerization, the bonding 

layer will be thicker and consist of a dense polymer matrix 

that promotes better sealing. 

Self-etching adhesives (except IBO) obtained higher 

dentin sealing capability than etch-and-rinse adhesives. To 

etch and infiltrate at the same time assures proper covering 

of the demineralized dentin and avoids the problem of water, 

which etch-and-rinse adhesives have after phosphoric 

etching. 4,11 The lower primer acidity promotes less tubule 

opening, 14 and then tubule sealing was demonstrated to be 

easier. 6 The consequence is that self-etching adhesives always 

sealed the dentin tubules and yielded lower leakage 

than etch-and-rinse adhesives. In accordance with others, 

6,15 IBO allowed more leakage than other adhesives tested. 

Despite the higher leakage, IBO sealed always the dentin 

tubules. 

Evaluation of the dentin permeability to the dye solution 

shows the adhesive ability to seal the dentin tubules. 16 Within 

the limits of a microleakage study (not being a nanoleakage 

evaluation), it can be concluded that if there is leakage 

but no positive permeability, the interface failure will be located 

over the intact dentin. In this situation, penetrating 

bacteria will be surrounded by resin interfaces which could 

slow down secondary caries development. In fact, pulp inflammation 

was measured in vivo, 12 and when the bacteria 

progressed between the cavity and the composite, a low level 

of pulp inflammation was found. However, if the bacteria 

progress into the dentin tubules, the inflammatory activity is 

higher. 3 Therefore, it is desirable to achieve sealing of dentinal 

tubules. 

Thermocycling is an easy method to age restorations and 

results in the highest clinically relevant stress. 3,18 As was 

demonstrated in others studies, 18 thermocycling did not af- 


Rosales-Leal 

fect the occlusal sealing and showed that the enamel junction 

is resistant to aging, due to the mineral nature of the tissue 

which ensures a better and more durable bond. 4 In contrast, 

the dentin bond was susceptible to damage and the 

sealing was reduced after thermocycling. 18 The larger proportion 

of organic compounds and water in the dentin 

makes the union weaker for all the adhesives tested, which 

would explain aging. 11,17 Thermocycling accelerates the aging 

by hydrolytic degradation of the hydrophilic components 

in the bonding system. 12,22 In addition, repetitive contraction/expansion 

stress at the bonding interface may lead to 

cracks that propagate along the interface and cause in- and 

outflow of fluids. 5 When considering distribution of microleakage 

grades in all obtained slices, only XPB was not 

affected by thermocycling. 

Clinically, when a cavity is surrounded by enamel, the 

phosphoric acid will ensure a hermetic and durable bond. 

When the cavity margins are in dentin, improvements are 

necessary, but there are some self-etching adhesives (XNO, 

CLF) or etch-and-rinse adhesives (XPB) that obtain excellent 

results with no positive dentin permeability and low leakage. 

Perhaps more acidic primers could improve the sealing of 

composite resin restorations. 

CONLUSIONS 

In enamel, no microleakage was found when phosphoric 

acid was used, but self-etching adhesives showed slight 

leakage. The gingival sealing was inferior to the occlusal 

sealing. XNO and CLF obtained the best gingival sealing, followed 

by XPB, SBX, P&B, and IBO, with SYN demonstrating 

the worst sealing. Self-etching adhesives and XPB were able 

to hermetically seal the dentin tubules (negative permeability). 

Thermocycling did not affect the occlusal bonding or XPB 

gingival sealing. 


This research was sponsored by Dentsply DeTrey, Konstanz, Germany. 

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17:296-308. 

20. Van Meerbeek B, InokoshiS, Braem M, Lambrechts P, Vanherle G. Morphological 

aspects of the resin-dentin interdiffusion zone with different dentin 

adhesive systems. J Dent Res 1992;71:1530-1540. 

21. Van Meerbeek B, Perdigão J, Lambrechts P, Vanherle G. The clinical performance 


22. Yang B, Adlung R, Ludwig K, Böbmann K, Pashley DH, Kern M. Effect of 

structural change of collagen fibrils on the durability of dentin boning. Biomaterials 

2005;26:5021-5031. 

REFERENCES 

1. de la Torre-Moreno FJ, Rosales-Leal JI, Bravo M. Effect of cooled composite 

inserts in the sealing ability of composite resin restorations placed at intraoral 

temperatures: an in vitro study. Oper Dent 2003;28:297-302. 


M, Van Meerbeek B. A Critical Review of the Durability of Adhesion to Tooth 

Tissue: Methods and Results. J Dent Res 2005;84:118-132. 

Clinical relevance: Phosphoric acid ensures hermetic 

and durable union on enamel. Although there are some 

excellent adhesives, it is nesessary to improve the 

dentin sealing. 


Sarrett 


Microleakage of XP Bond in Class II Cavities After 

Artificial Aging 

Jürgen Manhart a /Cordula Trumm b 

Purpose: To determine the microleakage of etch and rinse adhesives. 

Materials and Methods: Standardized Class II cavities were cut in 40 human molars with one proximal box limited 

within enamel and one proximal box extending into dentin. Teeth were assigned randomly to 5 groups (n = 8) and restored 

with incrementally placed composite restorations. Five combinations were tested: G1 = XP Bond + CeramX 

Mono, G2 = Syntac Classic + Tetric EvoCeram, G3 = Scotchbond 1 XT + Z250, G4 = P&B NT + CeramX Mono, G5 = 

Optibond Solo Plus + CeramX Mono. After finishing and polishing, teeth were stored for 48 h in water at 37°C before 

being subjected to artificial aging by thermal stress (5/55°C, 2000x, 30 s) and mechanical loading (50 N, 50,000x). 

Teeth were isolated with nail varnish and immersed in 5% methylene blue for 1 h. After sectioning, specimens were 

evaluated for leakage (ordinal scale: 0 to 4) at enamel and dentin margins under a stereomicroscope. Results were 

analyzed using the Kruskal-Wallis H-test and Mann-Whitney U-test (p < 0.05). 

Results: Statistical analysis showed significant differences among the groups in both enamel and dentin. Mean 

ranks (H-test) were: enamel: G2 (64.44) < G1 (66.69) < G4 (74.88) < G3 (98.25) and G5 (98.25); dentin: G3 (65.53) < 

G1 (74.42) < G4 (81.09) < G2 (81.84) < G5 (99.61). 

Conclusion: Microleakage of XP Bond is at the same level as or even better than other etch-and-rinse adhesives. 

Keywords: Class II restorations, dentin adhesives, composite, microleakage. 


Despite improvements in the formulation of modern 

dentin adhesive systems, the bond strength and marginal 

adaptation of composite resins to dentin seems still inferior 

and less predictable than adhesion to enamel. 3,11 

However, most of the cavities in clinical dentistry, especially 

when restorations in the posterior region of the mouth are 

replaced, are not limited exclusively within enamel but show 

a mixed type configuration with finishing lines in both enamel 

and dentin. 3,12 In particular, the adhesive interface between 

tooth and restorative material at the gingival finish 

line has been recognized as one of the most problematic regions. 

5,9 While a great number of self-etching primers and 

adhesives have emerged on the market, which are considered 

less technique sensitive and less time consuming than 

etch-and-rinse adhesives, 13 the latter are still considered 

the gold standard with respect to long-term bond strength 

and marginal seal, especially for the restoration of highly 

loaded Class II cavities or when restorations are bonded to 

uninstrumented tooth tissues such as sclerotic dentin in 

Class V lesions or virgin enamel in anterior diastema closures. 

This study assesses the microleakage of a newly formulated 

etch-and-rinse adhesive, based on a tert-butanol solvent 

used for the first time, in large Class II cavities after artificial 

aging in comparison with well-established competitive 

adhesive and composite systems. The null hypothesis tested 

was that the type of restorative system used does not significantly 

affect the marginal seal. 

a Associate Professor, Department of Restorative Dentistry, Ludwig Maximilians 

University, Munich, Germany. 

b Dentist in Private Practice, Munich, Germany. 



Reprint requests: Dr. Jürgen Manhart, Department of Restorative Dentistry, 

Goethe Street 70, 80336 Munich, Germany. Tel: +49-89-5160-7610, Fax: +49- 

89-5160-9302. e-mail: manhart@manhart.com 


Specimen Preparation 

Forty freshly extracted caries-free human permanent molars, 

stored in a 0.25% mixture of sodium azide in Ringer solution 

until the date of use, were used in this in vitro study. 

After cleaning the teeth with scalers and polishing with 


Manhart/Trumm 

Table 1 Experimental groups and materials used 

Group Adhesive Solvent type of Composite 

adhesive 

G1 XP Bond (Dentsply t-butanol Ceram-X Mono (M2) 

DeTrey; Konstanz, Germany 

(Dentsply DeTrey) 

G2 Syntac Classic Primer: acetone-water Tetric EvoCeram (A2) 

(Ivoclar Vivadent; Adhesive: water (Ivoclar Vivadent) 

Schaan, Lichtenstein Heliobond: - 

G3 Scotchbond 1 XT Ethanol-water Z250 (A2) 

(3M ESPE; Seefeld, Germany) (3M ESPE) 

G4 Prime & Bond NT (Dentsply Acetone Ceram-X Mono (M2) 

DeTrey; Konstanz, Germany 

(Dentsply DeTrey) 

G5 Optibond Solo Plus (Kerr-Hawe; Ethanol Ceram-X Mono (M2) 

Bioggio, Switzerland 

pumice, standardized Class II inlay cavities (MOD) were prepared, 

with one proximal box limited within enamel (1 to 1.5 

mm above the cementoenamel junction) and one proximal 

box extending into dentin (1 to 1.5 mm below the cementoenamel 

junction) (Fig 1). The cavities were 4.0 mm in width 

and 3 to 3.5 mm in depth at the occlusal isthmus and 5.0 

mm in width at the proximal boxes. The depth of the proximal 

boxes in the direction of the axial pulpal walls was 1.5 

mm. To achieve divergence angles between opposing walls 

of 10 to 12 degrees, cavities were prepared using coarse diamond 

burs with a slight taper (855.314, Komet; Lemgo, 

Germany) in a high-speed dental handpiece with copious water 

spray. Fine grained diamond burs of the same shape 

(8855.314, Komet) were used for finishing the preparations. 

The internal point and line angles were rounded and enamel 

margins were not beveled but prepared in butt-joint configuration. 

11 After visual inspection of the cavities for imperfect 

finish lines, the 40 prepared teeth were randomly assigned 

to 5 experimental groups with 8 teeth each (Table 1), 

corresponding to the different restorative techniques. Manufacturers' 

instructions for each material were strictly followed. 

For the direct composite restorations, all enamel and 

dentin surfaces of the cavities were conditioned with 36% 

phosphoric acid gel (DeTrey Conditioner 36, Dentsply De- 

Trey; Konstanz, Germany), starting acid application on enamel, 

leaving undisturbed for 15 s, then covering the dentinal 

preparation surfaces for an additional 15 s (total-etch technique). 

After thoroughly rinsing with water, the cavities were 

then gently dried with oil-free compressed air, taking care to 

avoid desiccation of the tooth substrate (moist bonding technique). 

Following the application and light curing of the adhesive 

systems, the cavities were restored with composite 

resin (Table 1) using a horizontal and oblique layering technique 

with 5 increments in the dentin-limited proximal box 

and 4 increments in the enamel-limited box (Fig 1). Each increment 

with a maximum thickness of 2 mm was light cured 

individually with a LED curing unit (SmartLite PS, Dentsply 

DeTrey) according to the manufacturer’s recommendations. 

The light output of the curing unit was monitored at 1065 

mW/cm 2 with a calibrated light meter (CureRite, Dentsply 

DeTrey). All restorations were finished and polished immediately 

after placement using finishing diamond burs and 

polishing disks (Sof-Lex, 3M ESPE; Seefeld, Germany). 

Thermocycling and Mechanical Loading 

After 48 h storage in distilled water at 37°C, the restored 

teeth were subjected to artificial aging by thermocycling and 

mechanical loading. All specimens were immersed alternately 

in water baths at 5°C and 55°C for 2000 cycles, with 

a dwell time of 30 s in each bath and a transfer time of 15 

s. Mechanical loading of the teeth, which were mounted on 

metallic specimen holders with a light-curing composite, was 

conducted in the Munich Oral Environment. 8 The carefully 

aligned teeth were loaded in the central fossa of the restorations 

in axial direction with a force of 50 N for 50,000 times 

at a frequency of 1 Hz. The antagonist material was a Degusit 

sphere 6 mm in diameter, which exhibits a hardness 

and wear resistance similar to natural enamel. 8,19-21 The 

metal specimen holders were mounted on a hard rubber element, 

which allowed a sliding movement of the tooth between 

the first contact on an inclined plane to the central 

fossa. 4 During mechanical loading, the teeth were continuously 

immersed in Ringer solution. This oral simulation device 

exhibits similar functions to the machine developed by 

Krejci. 7 

Evaluation of Microleakage 

The apices of the artificially aged teeth were sealed with adhesive 

and composite (Prime & Bond NT and Ceram-X 

Mono). All tooth surfaces were covered with 2 coats of nail 

varnish to within approximately 1 mm of the margin of the 

restoration. Microleakage was tested using a standardized 

dye penetration method. The specimens were immersed in 

5% methylene blue at 37°C for 1 hour and then rinsed with 

tap water. Teeth were embedded in clear acrylic auto-polymerizing 

resin (Technovit, Kulzer; Wehrheim, Germany). All 

restorations were sectioned longitudinally with two parallel 

cuts in three fragments in mesiodistal direction with a water-cooled 

low-speed diamond saw (Varicut, Leco; Kirch- 


Manhart/Trumm 

heim, Germany), resulting in four readings for each specimen 

at the enamel and dentin adhesive interface. An ordinal 

scale from 0 to 4 was used to score microleakage separately 

at the enamel and dentin margins of each section 

(Fig 2). 6 Each section was examined under a stereomicroscope 

(Stemi SV 11, Zeiss; Oberkochen Germany) at 40X 

magnification and scored by two examiners. Consensus was 

forced if disagreements occurred. 16 The results of the microleakage 

investigation were analyzed using the nonparametric 

Kruskal-Wallis H-test and post-hoc Mann-Whitney 

U-test at a significance level of p < 0.05. 

RESULTS 

Microleakage results are presented in Table 2. The Kruskal- 

Wallis H-test revealed statistically significant differences 

among the experimental groups in the enamel (p = 0.001) 

and dentin margins (p = 0.022) of the Class II restorations. 

DISCUSSION 

Microleakage studies provide adequate screening methods, 

possibly determining what kind of adhesive system will show 

acceptable clinical performance. 13 While quantitative marginal 

analysis by scanning electron microscopy assesses the 

entire circumference of the tooth/restoration interface, it can 

only determine the quality of the adhesive interface at the 

cavosurface margin. The extension of marginal gaps towards 

the axial wall of restorations is commonly assessed by microleakage 

studies. 10 Detection of microleakage can be accomplished 

with a number of techniques, including bacteria, 

chemical or radioactive tracer molecules, fluid permeability, 

and dye penetration. 1 The most common technique is the 

use of dyes, the penetration of which is determined after sectioning 

of the specimen with a magnifying aid. 

The type of solvent strongly influences the clinical application 

protocol of etch-and-rinse adhesive systems. Acetonebased 

systems only work well on a moist dentin surface as 

acetone is a water chaser and can lead to rather poor results 

on overdried acid-etched dentin surfaces. On the other 

Fig 1 Incremental restoration technique and light curing direction. 

11 

hand, water-based systems are not as sensitive with regard 

to dentin moisture content, as they have inherent rewetting 

properties, but require a longer evaporation time for the solvent, 

because water has a considerably lower vapor pressure 

than acetone. 18 If the solvent is not completely evaporated 

before light curing the adhesive, flaws can weaken the 

hybrid layer, probably causing premature restoration failure. 2 

A new type of solvent for adhesives, namely, tert-butanol, was 

introduced for XP Bond. Tert-butanol (2-methyl-2-propanol) 

Table 2 Microleakage frequency scores at enamel and dentin margins in the experimental groups G1 to G5. 

Enamel 

Dentin 

Leakage 0 1 2 3 4 Mean rank Leakage 0 1 2 3 4 Mean rank 

score (Kruskal- score (Kruskal- 

Wallis) 

Wallis) 

G1 28 0 4 0 0 66.69 a G1 20 3 4 5 0 74.4 A 

G2 28 3 1 0 0 64.44 a G2 18 1 7 4 2 81.84 A,B 

G3 15 7 9 1 0 98.25 b G3 23 5 1 2 1 65.53 A 

G4 24 4 4 0 0 74.88 a G4 19 2 2 7 2 81.09 A,B 

G5 15 7 9 1 0 98.25 b G5 10 6 7 6 3 99.61 B 

Different superscript letters indicate statistically significantly different subsets within each margin segment as determined by post-hoc 

multiple comparisons with the Mann-Whitney U-test (p < 0.05) 


Manhart/Trumm 

Fig 2 Scoring system for microleakage 

evaluation in enamel and dentin. 

consists of a C4 body with an alcohol group surrounded by 3 

methyl groups, making it totally miscible both with water and 

polymerizable resins. Although tert-butanol has a higher molecular 

weight than ethanol, the evaporation rate is almost the 

same, with a latent heat of vaporization of 41 kJ/mol for tertbutanol 

and 42 kJ/mol for ethanol. 15 Vapor pressure of the 

different kinds of solvents at 20°C is given as 2330 Pa for water, 

4133 Pa for tert-butanol, 5900 Pa for ethanol, and 

23,300 Pa for acetone. 14 The properties of tert-butanol make 

it possible to use a dappen dish and increase the resin content 

of the adhesive, which results in an increase of adhesive 

layer thickness and a higher degree of technique robustness 

as compared to acetone-based systems. The solvent used for 

etch-and-rinse adhesives is a major factor affecting handling 

characteristics and performance. 2,17 

CONCLUSIONS 

The two-step one-bottle tert-butanol-based XP Bond showed 

excellent microleakage results in both enamel and dentin, 

with the same quality as a well-established three-step etchand-rinse 

system. 

ACKNOWLEDGEMENTS 

This research was sponsored by Dentsply DeTrey, Konstanz, Germany 

. 

REFERENCES 

1. Alani AH, Toh CG. Detection of microleakage around dental restorations: a 

review. Oper Dent 1997;22:173-185. 


M, Van Meerbeek B. A critical review of the durability of adhesion to tooth 

tissue: methods and results. J Dent Res 2005;84:118-132. 

3. Dietrich T, Lösche AC, Lösche GM, Roulet JF. Marginal adaptation of direct 

composite and sandwich restorations in Class II cavities with cervical margins 

in dentine. J Dent 1999;27:119-128. 

4. Dietschi D, Herzfeld D. In vitro evaluation of marginal and internal adaptation 

of class II resin composite restorations after thermal and occlusal 

stressing. Eur J Oral Sci 1998;106:1033-1042. 

5. Dietschi D, Scampa U, Campanile G, Holz J. Marginal adaptation and seal 

of direct and indirect class II composite resin restorations: An in vitro evaluation. 

Quintessence Int 1995;26:127-138. 

6. Hilton TJ, Ferracane JL. Cavity preparation factors and microleakage of 

class II composite restorations filled at intraoral temperatures. Am J Dent 

1999;12:123-130. 

7. Krejci I, Reich T, Lutz F, Albertoni M. In-vitro-Testverfahren zur Evaluation 

dentaler Restaurationssysteme. 1. Computergesteuerter Kausimulator. 

Schweiz Monatsschr Zahnmed 1990;100:953-960. 

8. Kunzelmann KH. Verschleissanalyse und -quantifizierung von Füllungsmaterialien 

in vivo und in vitro. Aachen: Shaker-Verlag 1998. 

9. Lutz F, Kull M. The development of a posterior tooth composite system, invitro 

investigation. Schweiz Monatsschr Zahnmed 1980;90:455-483. 

10. Manhart J, Chen HY, Mehl A, Weber K, Hickel R. Marginal quality and microleakage 

of adhesive class V restorations. J Dent 2001;29:123-130. 

11. Manhart J, Hollwich B, Mehl A, Kunzelmann KH, Hickel R. Randqualität von 

Ormocer- und Kompositfüllungen in Klasse-II-Kavitäten nach künstlicher Alterung. 

Dtsch Zahnärztl Z 1999;54:89-95. 

12. Mayer R. Ästhetisch-adhäsive Füllungstherapie im Seitenzahngebiet - eine 

Illusion Dtsch Zahnärztl Z 1991;46:468-470. 

13. Owens BM, Johnson WW, Harris EF. Marginal permeability of self-etch and 

total-etch adhesive systems. Oper Dent 2006;31:60-67. 

14. Roempps Chemie-Lexikon. 8th Edition, Stuttgart: Franckh-Fachlexikon 

1981. 

15. Scientific Compendium: XP Bond universal total-etch adhesive. Konstanz: 

DENTSPLY DeTrey 2006. 

16. Swift EJ, Triolo PT, Barkmeier WW, Bird JL, Bounds SJ. Effect of low-viscosity 

resins on the performance of dental adhesives. Am J Dent 1996;9:100- 

104. 

17. Tay FR, Gwinnett AJ, Wei SHY. Relation between water content in acetone / 

alcohol based primer and interfacial ultrastructure. J Dent 1998;26:147- 

156. 

18. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van 

Landuyt K, Lambrechts P, Vanherle G. Adhesion to enamel and dentin: Current 

status and future challenges. Oper Dent 2003;28:215-235. 

19. Wassell RW, McCabe JF, Walls AWG. Subsurface deformation associated 

with hardness measurements of composites. Dent Mater 1992;8:218- 

223. 

20. Wassell RW, McCabe JF, Walls AWG. A two-body frictional wear test. J Dent 

Res 1994;73:1546-1553. 

21. Wassell RW, McCabe JF, Walls AWG. Wear characteristics in a two-body 

wear test. Dent Mater 1994;10:269-274. 

Clinical relevance: The new tert- butanol- based XP 

Bond is expected to show good clinical results due to its 

chemical composition and technique robustness. 


Six-month Clinical Evaluation of XP BOND in Noncarious 

Cervical Lesions 

Uwe Blunck a /Katharina Knitter b /Klaus-Roland Jahn c 

Purpose: To evaluate the 6-month clinical performance of the etch-and-rinse one-bottle adhesive system XP BOND, 

used in combination with the composite resin CeramX Duo for the restoration of Class V noncarious cervical lesions 

(NCCL). 

Materials and Methods: XP BOND was tested in a total of 40 patients who received two Class V CeramX Duo restorations, 

Adper Scotchbond 1 XT was used as a control. After cleaning the teeth, the surface of the NCCL was treated 

using a carbide bur in dentin and a 40-μm diamond bur in enamel with no retentive preparations. The lesions were 

filled with two increments of CeramX Duo after the application of the respective adhesive by a single operator according 

to manufacturer’s instructions. After 6 months, the retention and the marginal integrity were evaluated. 

Results: Thirty-eight of 40 patients were evaluated after 6 months by two clinicians according to modified USPHS criteria, 

and all restorations using XP BOND were still in place. In the control group (using Adper Scotchbond 1XT), one 

restoration was lost. The statistical evaluation (chi 2 test) showed no significant differences in any of the criteria. No 

difference of marginal integrity was found between the two adhesive systems. 

Conclusion: XP BOND meets the ADA success criteria after 6 months. 

Keywords: clinical study, noncarious cervical lesions, Class V restorations, adhesive systems. 

J Adhes Dent 2007; 9:265-268. Submitted for publication: 15.12.06x; accepted for publication: 3.1.07. 

In operative dentistry, etch-and-rinse systems form an important 

group of bonding agents that are clinically widely 

used. However, as these systems require the demineralization 

of dentin and the exposure of the embedded collagen 

network, numerous concerns regarding drying of the protein 

mesh arise. 5,6,8 This is due to the need to rinse and carefully 

a Associate Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus 

Virchow Clinic, Berlin, Germany. 

b Assistant Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus 

Virchow Clinic, Berlin, Germany. 

c Professor, Charité-Universitätsmedizin Berlin, Dental School, Campus Virchow 

Clinic, Berlin, Germany. 



Reprint requests: Dr. Uwe Blunck, Charité-Universitätsmedizin Berlin, Dental 

School, Campus Virchow Clinic, Augustenburger Platz 1, 13353 Berlin, Germany. 

Tel: +49-30-450-562-673, Fax: +49-30-450-562-961. e-mail: 

uwe.blunck@charite.de 

dry the surface after acid etching, in order to enable the constituents 

of the bonding system, specifically the uncured 

monomers, to penetrate the outer layers of the prepared 

dentin. It has therefore been proposed that a bonding system 

capable of penetrating dry and collapsed demineralized 

dentin would improve bonding, resulting in better clinical 

performance. 8 

XP BOND is a new one-bottle etch-and-rinse adhesive, 

composed of a pre-mixed solution of monomers dissolved in 

tert-butanol. Due to an improved ability to diffuse through 

partially collapsed demineralized dentin, it is claimed to be 

less technique sensitive. 2 

As for any other new dental restorative, data from clinical 

investigations are crucial to assess the effectiveness and reliability 

of the product before being launched. This is needed 

in order to validate results from the in vitro studies. As 

generally accepted for investigating the clinical effectiveness 

of such adhesive systems, noncarious Class V restorations 

are the standard test. 9,13 This is due to the fact that 

they do not provide any macromechanical retention, they require 

at least 50% bonding to dentin, and they are widely 


Blunck et al 

Table 1 Materials used in the study 

Material Manufacturer Batch No/expiration date 

XP BOND Dentsply 0512004001/2006-07 

(K-0127.04) 

Adper 3M ESPE 214747/2007-04 

Scotchbond 

1 XT 

Ceram•X Duo Dentsply D1: 0119 

D2: 1617 

D3: 0174 

D4: 0116 

DB: 1381 

E1: 0583 

E2: 2507 

E3: 2624 

2008-03 

seen. Adper Scotchbond 1 XT was applied as recommended 

for 15 s in 2 or 3 layers, then carefully dried for at least 5 

s, resulting in a glossy surface. Both adhesives were light 

cured for 10 s (Smartlite PS, Dentsply DeTrey) before the application 

of CeramX Duo in at least two increments (depending 

on the extension of the cervical lesion); each increment 

was light cured for 40 s. The restorations were then finished 

and polished by using the PoGo (Dentsply DeTrey) polishing 

system. 

The patients were recalled after 3 and 6 months. The 

restorations were checked by two evaluators. The criteria of 

interest were retention, postoperative sensitivity, marginal 

discoloration, margin integrity, secondary caries, and contour, 

using the modified USPHS criteria. 1,17 A vitality test was 

performed and the color match of the restoration with the 

surrounding tooth structure was also evaluated by the patients. 

RESULTS 

available, usually found in anterior teeth or premolars with 

good access for easy restoring and evaluation. 

The purpose of this investigation was to evaluate the effectiveness 

of XP BOND compared to Adper Scotchbond 1 

XT when used to restore noncarious cervical lesions, both 

materials being applied with the etch-and-rinse technique. 


In 40 patients bearing noncarious cervical lesions (NCCL), 

80 Class V restorations were placed with either XP BOND or 

Adper Scotchbond 1 XT (Table 1). Both agents were used according 

to manufacturer’s instructions, combined with the 

composite resin CeramX Duo, and completed by a single operator. 

The patients (age range 24 to 77, 17 females and 23 

males) were all treated within the framework of the student 

courses of the Charité Dental School in Berlin, Campus Virchow 

Clinic. The reasons for treatment were esthetic considerations, 

hypersensitive cervical dentin, or prevention of 

further erosion. The agreement for voluntary participation 

and informed consent were obtained prior to treatment. Approval 

for this study was given by the Ethics Committee of the 

Charité Berlin (EA2/230/05, Protocol-Nr.: 14.1165). 

Each lesion was initially cleaned with a nonfluoridated 

polishing paste (Pellex, KerrHawe; Bioggio, Switzerland) on 

a slowly rotating rubber cup, washed, and slightly dried. The 

dentin surface was treated using a carbide bur (air cooled) 

and the enamel margins were trimmed with a 40-μm diamond 

bur under water spray. Saliva control was maintained 

by cotton rolls. For both adhesive systems, 36% phosphoric 

acid (DeTrey Conditioner 36, Dentsply DeTrey; Konstanz, 

Germany) was used for standard etching (30 s on enamel 

and then 15 s on dentin). After rinsing for at least 15 s, the 

cavity was carefully dried without desiccating the dentin. A 

single layer of XP BOND was applied for 20 s and the solvent 

was evaporated for at least 5 s until a glossy surface was 

As seen from the results listed in Table 2, 6 months after 

placement, 38 out of 40 patients were available for recall. 

All restored teeth were still in contact with their antagonists 

(checked during laterotrusion) with 60% showing active wear 

facettes. All restorations placed with XP BOND were still in 

place and showed no marginal discoloration, while in the 

control group, one restoration was lost and two (5.4%) 

showed discoloration of less than 50% of the margin length. 

In neither group were visible margin irregularities found, and 

the margins were not detectable with a dental probe. No secondary 

caries and no surface staining were noted. With XP 

Bond, one restored tooth showed postoperative hypersensitivity 

after 6 months, while in the control group, two teeth 

were hypersensitive. 

Chi 2 tests were performed using the SPSS (SPSS 12.0 for 

Windows, SPSS; München, Germany) statistical package. 

We found no significant differences for the different criteria 

between the test XP BOND and the control adhesive. 

DISCUSSION 

Within the limitations of a 6-month clinical study, our data 

clearly show the favorable results for XP BOND. The retention 

of all restorations of the treated NCCLs and the lack of staining 

at the margins, combined with ease of use, show much 

promise for similar and other types of restorations as well. 

This study, performed in accordance with manufacturer’s instructions, 

did not attempt to test this product under extreme 

desiccation conditions, for which it is presumed to 

have an advantage. 2 Rather, our work was used to assess 

the clinical performance of XP BOND under “normal”, reasonable 

clinical conditions. 

This study was designed to test XP BOND under a rather 

well-defined clinical challenge: the treatment of NCCLs. 

Class V restorations, used to treat this type of lesion, are a 

reasonable choice for a clinical evaluation of a new adhesive 

system because the bonding efficacy and handling characteristics 

are exposed to a realistic and trying intraoral situa- 


Blunck et al 

Table 2 Results of the clinical assessment in% of the modified USPH criteria 

Criteria for XP BOND [%] Adper Scotchbond 1XT [%] 

evaluated 

restorations n alpha bravo charlie delta n alpha bravo charlie delta 

Retention 38 100 0 0 0 38 97.4 0 0 2.6 

Postoperative 38 97.4 2.6 0 0 37 94.6 5.4 0 0 

sensitivity (∑) 

Marginal 38 100 0 0 0 37 94.6 5.4 0 0 

discoloration 

Marginal 38 100 0 0 0 37 100 0 0 0 

integrity 

Secondary 38 100 0 0 0 37 100 0 0 0 

caries 

Restoration 38 100 0 0 0 37 100 0 0 0 

contour 

Vitality test 38 100 0 0 0 37 100 0 0 0 

tion. A variety of factors, such as the nutrition of the patient, 

parafunction, chewing habits, oral hygiene etc, modify the 

dentin surface such that the morphology and microstructure 

are different compared to surfaces that are exposed during 

cavity preparation. 12 Thus, tubules of cervical dentin are exposed 

to the oral environment for a longer period and are frequently 

partially or totally occluded with precipitates. This 

forms a hypermineralized dentin layer that has been found 

to be more resistant to etching. 4,10 As a result, a thinner hybrid 

layer is formed on the surface, which is different from 

the situation in noncervical, cut dentin. 12 It has been shown 

that the etch-and-rinse technique results in higher bond 

strengths than self-etching adhesive systems. 11 However, 

etching dentin with phosphoric acid involves a sensitive 

step, namely, the careful drying of the exposed collagen network. 

5 This network has to be penetrated completely when 

the adhesive system is applied. The results of this study suggest 

that XP BOND can produce an effective bond, which is 

reflected by the lack of discoloration and the retention results, 

as judged by two experienced dentists who have considerable 

experience with similar, previous clinical studies. 

An additional advantage of the use of a model based on 

the treatment of NCCLs is that Class V restorations minimize 

the influence of the operator variability. They also simplify 

the evaluation procedure of margin integrity, owing to the direct 

accessibility during the study period. 9,13 We note, however, 

that the margins of Class V restorations cover both 

enamel and dentin, and this might increase the retention 

due to bonding to the acid-etched enamel. Consequently, 

failure might develop due to reduced adhesion to dentin, 

which is less suited to withstand mechanical stress during 

mastication. Our evaluation of marginal staining and probing 

as well as the evaluation of hypersensitivity was aimed 

at identifying failures of this type; none were found. 

This evaluation is one part of a multicenter study. At present, 

the results after 6 months of an identical in vivo study 

at the University of Bologna, with 30 patients are available. 

The criteria retention, marginal discoloration, margin integrity, 

secondary caries, and restoration contour (Table 3) 

were all highly rated (alpha USPHS rating) for restorations in 

the XP BOND group, where only one restoration (3.3%) exhibited 

postoperative sensitivity. In the group using Adper 

Scotchbond 1 XT, all criteria received a 100% alpha rating, 

with postoperative sensitivity occurring in 7 teeth (23.3%) 

with a bravo USPHS rating. 

CONCLUSION 

It should be borne in mind that these results are preliminary. 

Further studies, which are to include other cavity designs 

and longer observation periods, can only help to establish 

the long-term reliability and the effect on the margin integrity 

of the oral environment. However, from the present study, 

it can be concluded that the results for the one-bottle etchand-rinse 

adhesive system XP BOND meet the criteria for a 

provisional acceptance according to ADA guidelines, with 

less than 5% failure rate after 6 months of clinical performance. 


This study was funded by Dentsply DeTrey, Konstanz, Germany. 


Blunck et al 

Table 3 Reference data obtained from the clinical assessment in % of the modified USPH criteria from the study center, 

Bologna 

Criteria for XP BOND [%] Adper Scotchbond 1XT [%] 

evaluated 

restorations n alpha bravo charlie delta n alpha bravo charlie delta 

Retention 30 100 0 0 0 30 100 0 0 0 

Postoperative 

sensitivity (∑) 30 96.7 3.3 0 0 30 76.7 23.3 0 0 

Marginal 30 100 0 0 0 30 100 0 0 0 

discoloration 

Marginal 30 100 0 0 0 30 100 0 0 0 

integrity 

Secondary 30 100 0 0 0 30 100 0 0 0 

caries 

Restoration 30 100 0 0 0 30 100 0 0 0 

contour 

Vitality test 30 100 0 0 0 30 100 0 0 0 

REFERENCES 

1. Barnes DM, Blank LW, Gingell JC, Gilner PP. A clinical evaluation of a resinmodified 

glass ionomer restorative material. J Am Dent Assoc 1995; 

126:1245-1253. 

2. Dentsply XP BOND for eXtra Performance. Scientific Compendium. Konstanz: 

Dentsply DeTrey, 2006. 

3. Dondi Dall'Orologio G. 6-Month report: clinical evaluation of the adhesive 

XP BOND for restoration of cervical lesions at the University of Bologna, 

Italy. Report to Dentsply 2006. 

4. Harnirattisai C, Inokoshi S, Shimada Y, Hosoda H. Adhesive interface between 

resin and etched dentin of cervical erosion/abrasion lesions. Oper 

Dent 1993;18:138-143. 

5. Kanca J. Resin bonding to wet substrate. I. Bonding to dentin. Quintessence 

Int 1992;23:39-41. 

6. Kanca J. Wet bonding: effect of drying time and distance. Am J Dent 

1996; 9:273-276. 

7. Loguercio AD, Reis A, Barbosa AN, Roulet JF. Five-year double-blind randomized 

clinical evaluation of a resin-modified glass ionomer and a polyacid-modified 

resin in noncarious cervical lesions. J Adhes Dent 2003; 

5:323-332. 

8. Peireira GDS, da, Paulillo LAMS, de Goes MF, Dias CTS. How wet should 

dentin be Comparison of methods to remove excess water during moist 

bonding. J Adhes Dent 2001;3:257-264. 

9. Peumans M, Kanumilli P, De Munck J, Van Landuyt K, Lambrechts P, Van 

Meerbeek B. Clinical effectiveness of contemporary adhesives: a systematic 

review of current clinical trials. Dent Mater 2005;21:864-881. 

10. Sakoolnamarka R, Burrow MF, Prawer S, Tyas MJ. Micromorphological investigation 

of noncarious cervical lesions treated with demineralizing 

agents. J Adhes Dent 2000;2:279-287. 

11. Tay FR, Kwong SM, Itthagarun A, King NM, Yip HK, Moulding KM, Pashley 

DH. Bonding of a self-etching primer to non-carious cervical sclerotic 

dentin: Interfacial ultrastructure and microtensile bond strength evaluation. 

J Adhes Dent 2000;2:9-28. 

12. Tay FR, Pashley DH. Resin bonding to cervical sclerotic dentin: a review. J 

Dent 2004;32:173-196. 

13. Van Meerbeek B, Perdigao J, Lambrechts P, Vanherle G. The clinical performance 



Adhesive Luting Revisited: Influence of Adhesive, 

Temporary Cement, Cavity Cleaning, and Curing Mode 

on Internal Dentin Bond Strength 

Roland Frankenberger a /Ulrich Lohbauer b /Michael Taschner c /Anselm Petschelt d / 

Sergej A. Nikolaenko e 

Purpose: To evaluate microtensile bond strength to Class I cavity floor dentin beneath adhesive inlays that were luted 

with different adhesives, temporary cements, cleaning methods, and curing modes. 

Materials and Methods: Occlusal cavities (4 x 4 mm, depth 3 mm) were prepared in 96 extracted human third molars. 

One part of the cavities was temporized with different temporary cements, which were removed after one week 

using three techniques (scaler or air polishing with Prophypearls or ClinPro powder). Direct resin composite inlays 

(Clearfil AP-X) were then placed with the luting composite Calibra using three adhesives (XP BOND/SCA, Syntac, Opti- 

Bond FL). Teeth were cut into beams and after 24 h of water storage at 37°C, the sticks were subjected to microtensile 

bond strength evaluation. Samples were subjected to SEM fractographic analysis of failed interfaces. 

Results: Contamination with temporary cement reduced dentin bond strengths (p < 0.05). Removing remnants of cements 

with Prophypearls air polishing resulted in the lowest bond strengths (p < 0.05). Separate light curing of the adhesives 

did not produce higher dentin bond strengths (p > 0.05). Syntac still worked when Heliobond was omitted (p > 

0.05). Immediate dentin sealing prior to temporizing increased internal bond strength (p < 0.05). 

Conclusion: The dual-cured adhesive provided higher internal bond strengths between adhesive inlays and dentin. Contamination 

of dentin with temporary cements is a hazard for excellent dentin adhesion of adhesive inlays. Therefore, immediate 

dentin sealing and resin coating is promising. 

Keywords: etch-and-rinse, dentin bonding, adhesive inlays, microtensile bond strength. 


a Associate Professor, Dental Clinic 1, Operative Dentistry and Periodontology, 

University of Erlangen-Nuremberg, Erlangen, Germany. 

b Assistant Professor, Dental Clinic 1, Operative Dentistry and Periodontology, 


c Assistant Professor, Dental Clinic 1, Operative Dentistry and Periodontology, 


d Professor and Chairman, Dental Clinic 1, Operative Dentistry and Periodontology, 


e Professor and Head, Department of Operative Dentistry, Krasnojarsk State 

Medical Academy, Krasnojarsk, Russia. 



Reprint requests: Prof. Dr. Roland Frankenberger, Dental Clinic 1, Operative 

Dentistry and Periodontology, University of Erlangen-Nuremberg, Glueckstrasse 

11, D-91054 Erlangen, Germany. Tel: +49-9131-853-3693, Fax: +49-9131-853- 

Adhesive inlays have proven to be durable in the oral cavity. 

4,6,15,18,19,24,25,27,28 Clinical reports refer to bulk fractures 

as the main failure reason for all ceramic inlay systems. 

8-10,15,18,19,26 Clinical trials focusing on ceramic inlays 

reveal a certain deterioration of marginal quality; 7 however, 

when adhesive inlays are totally bonded to enamel and 

dentin, internal dentin bond strength is also an interesting 

factor for both stabilization and reduction of postoperative 

hypersensitivity. 14,15,20 

It is still not fully understood which mode of luting is most 

reliable for bonding adhesive tooth-colored inlays to enamel 

and dentin, but conventional etch-and-rinse systems with 

dual-cured resin composites seem to be the gold standard 

for luting. 1,15,18,20,16 

Therefore, the aim of the present in vitro study was to evaluate 

the performance of different etch-and-rinse adhesives 


Frankenberger et al 

Table 1 Overview of materials under investigation 

Adhesive + 

resin composite 

XP BOND/SCA + 

Calibra 

Syntac 

(with Calibra) 

OptiBond FL 

(with Calibra) 

Components 

Etchant: 36% phosphoric acid 

Primer/Bond: TCB resin, PENTA, UDMA, TEG-DMA, BHT, CQ, functionalized 

nanofiller; mixed with SCA (self-curing activator) 

Luting composite: 

Base: bis-GMA, EBPADM, silica, UDMA, TEG-MA, butylhydoxitoluol, barium 

glass, silica 

Catalyst: bis-GMA, EBPADM, silica, UDMA, TEG-MA, butylhydoxitoluol, benzoyl 

peroxide, barium glass, silica 

Etchant: 35% phosphoric acid 

Primer: maleic acid 4%, TEG-DMA, water, acetone 

Adhesive (2nd primer): water, PEG-DMA, glutaraldehyde 

Heliobond: bis-GMA, UDMA, TEG-DMA 

Luting composite: see above 

Etchant: 37.5% phosphoric acid 

Primer: HEMA, GPDM, MMEP, ethanol, water, initiators 

Adhesive: bis-GMA, HEMA, GPDM, barium-aluminum borosilicate glass, 

disodium hexafluorosilicate, fumed silica (total=48% filler) 

Luting composite: see above 

Manufacturer 

Dentsply DeTrey; Konstanz, 

Germany 

Ivoclar Vivadent; Schaan, 

Liechtenstein 

Kerr; Orange, CA, USA 

for luting of Class I resin composite inlays after different 

contaminations, temporary cement removal, and curing 

modes. The null hypothesis was twofold, that (1) different 

adhesives with different curing modes, and (2) different 

temporary cements and cleaning methods would have no 

influence on dentin bond strength beneath adhesively luted 

inlays. 


Ninety-six intact, noncarious, unrestored human third molars 

were stored in an aqueous solution of 0.5% chlora 

mine T at 4°C for up to 30 days. The teeth were debrided of 

residual plaque and calculus, and examined to ensure that 

they were free of defects under a light microscope at 20X 

magnification. Standardized Class I cavity preparations (4 

mm in width and length, 3 mm in depth) were performed. 

Cavities were cut using coarse diamond burs under profuse 

water cooling (80 μm, Two-Striper Prep-Set, Premier; St Paul, 

MN, USA), and finished with a 25-μm finishing diamond. Inner 

angles of the cavities were rounded and the margins 

were not bevelled. To guarantee a rectangular relation between 

the bonded interface and the direction of the later-cut 

μTBS beam, the cusps were flattened by 2 mm and then the 

cavity floor was prepared parallel to the flattened cusps. 

Direct resin composite inlays (Clearfil AP-X, Kuraray; 

Tokyo, Japan) were manufactured under isolation of the cavities 

with glycerine gel. The inlays received a cubic shape 

with the surface being parallel to the bottom of the cavity to 

facilitate positioning of the light-curing tip. The bottom sides 

of the inlays were sandblasted with aluminum oxide (Rondoflex 

27 μm, KaVo; Biberach, Germany), washed with 70% 

ethanol, and dried. The prepared teeth received provisional 

restorations (Fermit N, Ivoclar Vivadent; Schaan, Liechtenstein), 

and were stored in distilled water at 37°C for one 

week. The provisional restorations were either inserted with 

or without two different temporary cements (Temp Bond / 

Temp Bond NE, Kerr; Orange, CA, USA). Two more groups 

with hybridizing dentin prior to temporizing were also made, 

either with one coat of adhesive (immediate dentin sealing 17 

[IDS]) or with one 0.5-mm layer of flowable resin composite 

(X-Flow, Dentsply DeTrey; Konstanz, Germany) (resin coating 

technique 13 [RC]). Here, temporary cements were omitted 

because they play no role in bonding to dentin. 

After removing Fermit, cement remnants were removed 

with a scaler or using different air-polishing powders (Prophypearls 

Powder, KaVo; ClinPro Prophy Powder, 3M ESPE; 

Seefeld, Germany), both operating in a Prophyflex air-polishing 

device (KaVo) at the level of the occlusal cavity margin 

for 10 s. 2 After rinsing with tap water and drying, the cavities 

were treated with different adhesives and one luting 

composite (Table 1). Internal surfaces of the resin composite 

inlays were silanized with Monobond S (Ivoclar Vivadent), 

dried, and covered with the respective adhesive, which was 

not light cured. Adhesives and luting resin composite were 

polymerized with a Translux CL light-curing unit (Heraeus 

Kulzer; Dormagen, Germany). The intensity of the light was 

checked periodically with a radiometer (Demetron Research; 

Danbury, CT, USA) to ensure that 600 mW/cm 2 was always 

exceeded during the experiments. Adhesives were light 

cured for 40 s in the case where the protocol advised it. Oth- 



Table 2 Results of μTBS investigation to cavity floor dentin 

Adhesive 

Dentin 

contamination 

Cleaning 

method 

Curing mode 

of adhesive 

μTBS 

to cavity floor 

dentin in MPa (SD) 

XP BOND / SCA 

--- 

--- 

--- 

--- 

Temp Bond 

Temp Bond 

Temp Bond 

Temp Bond NE 

Temp Bond NE 

Temp Bond NE 

--- 

--- 

--- 

--- 

Scaler 

Prophypearls 

Clinpro powder 

Scaler 

Prophypearls 


No LC 

separate 

IDS 

RC 

no LC 

no LC 

no LC 

no LC 

no LC 

no LC 

39.6 (26.6) 

36.3 (19.2) 

38.4 (13.6) 

53.9 (17.1) 

21.9 (20.7) 

10.0 (14.9) 

34.5 (8.1) 

27.3 (16.2) 

11.0 (14.9) 

36.3 (20.5) 

Syntac 

--- 

--- 

--- 

--- 

--- 

Temp Bond 

Temp Bond 

Temp Bond 

Temp Bond NE 

Temp Bond NE 

Temp Bond NE 

--- 

--- 

--- 

--- 

--- 

Scaler 

Prophypearls 


Scaler 

Prophypearls 


No LC 

separate 

IDS 

RC 

w/o adhesive 

no LC 

no LC 

no LC 

no LC 

no LC 

no LC 

13.7 (15.7) 

19.0 (14.2) 

30.1 (15.9) 

47.9 (18.0) 

22.5 (14.3) 

9.7 (8.9) 

5.9 (6.5) 

12.1 (11.4) 

7.1 (10.3) 

4.1 (5.1) 

12.0 (8.9) 

OptiBond FL 

--- 

--- 

--- 

--- 

--- 

Temp Bond 

Temp Bond 

Temp Bond 

Temp Bond NE 

Temp Bond NE 

Temp Bond NE 

--- 

--- 

--- 

--- 

--- 

Scaler 

Prophypearls 


Scaler 

Prophypearls 


No LC 

separate 

IDS 

RC 

w/o adhesive 

no LC 

no LC 

no LC 

no LC 

no LC 

no LC 

19.2 (16.3) 

26.6 (13.8) 

37.7 (16.9) 

50.7 (17.8) 

24.0 (17.5) 

10.4 (9.5) 

6.5 (6.5) 

18.2 (12.6) 

8.3 (10.2) 

8.2 (10.5) 

22.1 (18.0) 

IDS=immediate dentin sealing; RC=resin-coating technique 

erwise, the luting composites were cured together with the 

adhesives with an occlusal curing time of 220 s. 

The peripheral areas of the reconstructed/filled teeth 

were removed, remaining specimens were sectioned into 

slices in an apical direction, which were sectioned again to 

yield resin-dentin beams. The saw was adjusted to steps of 

1 mm, due to the thickness of the blade (300 μm) resulting 

in sticks with a cross-sectional area of 700 x 700 μm (0.5 

mm 2 ). From the resulting sticks of each group, 20 were selected 

(n = 20). These 20 sticks had to have a remaining 

dentin thickness to the pulp of 2.0 ± 0.5 mm. If more than 

20 beams were collected with the correct remaining dentin 

thickness, 20 sticks were randomly selected. For the case 

that one or more of the selected sticks failed due to the sectioning 

process, the percentage of prematurely failed specimens 

in relation to the total number of selected specimens 

was recorded. If more than 20 beams were collected with 

the correct remaining dentin thickness, 20 sticks were randomly 

selected. For the case that one or more of the selected 

sticks failed due to the sectioning process, the failed 

specimens received 0 MPa as final μTBS result. 38 The μTBS 

sticks were stored in distilled water for 24 h at 37°C and then 

fractured according to a well-suited protocol. 3 Fractured interfaces 

were submitted to SEM (Leitz ISI 50, Akashi; Tokyo, 

Japan; sputtering with Balzers SCD; Balzers, Liechtenstein). 

Statistical analysis was performed using SPSS, Version 

14.0 for Windows XP (SPSS; Chicago, IL, USA). As the majority 

of groups did not exhibit normal data distribution (Kolmogorov-Smirnov 

test), nonparametric tests were used 

(Wilcoxon matched-pairs signed-ranks test, Mann-Whitney 

U-test) for pairwise comparisons at the 95% significance 

level. 



Fig 1 Fractured μTBS specimen at the resin composite aspect 

with Syntac not separately cured. Short resin tags have been 

pulled out of the dentin at the cavity floor. 

Fig 2 Fractured μTBS specimen with XP Bond + SCA at the 

dentin side. The interface is ruptured at the bottom of the hybrid 

layer at the transition to the funnel-shaped orifices of dentinal 

tubules. 

RESULTS 

The results of the study are displayed in Table 2. Contamination 

with temporary cement reduced dentin bond 

strengths (p < 0.05). Removing remnants of cements with 

Prophypearls air-polishing significantly decreased dentin 

bond strengths (p < 0.05). Separate light curing of the adhesives 

did not produce higher dentin bond strengths (p > 

0.05). The dual-cured adhesive exhibited significantly higher 

bond strengths in control groups without IDS (p < 0.05). 

Immediate dentin sealing (resin coating) prior to temporizing 

increased internal bond strength for all adhesives under investigation 

(p < 0.05). Fractographic analysis exhibited insufficient 

interface formation when light-cured adhesives 

were cured together with the luting resin composite (Fig 1). 

Fractured interfaces of XP Bond showed characteristic positive 

features of typical etch-and-rinse adhesives (Fig 2). 

DISCUSSION 

The survival of ceramic inlays is fundamentally dependent 

on durable enamel bonding; also when the dentin aspects 

were covered with a cement lining, long-term success was reported 

to be good. 4,14-16 However, the present study exclusively 

focussed on internal dentin bond strength beneath adhesive 

inlays. Due to easier processing, direct resin composite 

inlays were chosen, because they reveal the same 

dentin-resin composite interface as ceramic inlays. 12,13,16,29 

Hikita et al 11 evaluated enamel and dentin bond 

strengths of luting systems for adhesive inlays. It was remarkable 

that Syntac and Variolink II without separate light 

curing of the adhesive obtained the lowest dentin bond 

strengths in that investigation. This may be surprising, because 

especially this combination of light-curing adhesive 

and dual-curing luting resin composite has been repeatedly 

reported to be clinically effective. 4,14,15 This clearly demonstrates 

that the clinical success of ceramic inlays as well as 

of direct resin composite restorations may be primarily dependent 

on good and durable marginal adaptation to enamel. 

The present results also clearly confirm the theory that 

solely light-cured adhesives do not receive enough light energy 

through 3-mm-thick adhesive inlays, not even under laboratory 

conditions. To elucidate the problem of insufficient 

light curing through ceramic inlays as demonstrated in vitro, 

marginal quality assessment alone is not sufficient. A previous 

and often cited study with conical ceramic inserts luted 

into standardized dentin cavities showed good bond 

strengths and marginal adaptation in vitro, even when the 

light-curing adhesive was not light cured separately. 5 However, 

in the course of push-out investigations, in most of the 

cases, enough light energy passes through the specimens, 

being considerably thinner than inlay cavities. Previous results 

showed that enough light intensity was always transported 

to the marginal areas of the luted ceramic inays, 

even in proximal margins below the CEJ. 1 Nevertheless, this 

does not necessarily mean that the light-curing adhesives 

under investigation revealed a complete cure in all areas beneath 

the ceramic inlays. The present results clearly show 

that results of marginal analyses may produce results which 

are not representative for what is happening deeper inside 

the restored tooth. 

In this context, it has often been discussed in the past 

whether a light-cured adhesive has to be separately light 

cured prior to the application of a luting resin composite. 

This study indicates that a separate light-curing step of lightcured 

adhesives was not beneficial for dentin bond strength. 

This may be attributed to the fact that heavily air-thinned layers 

of bonding agents are subjected to severe oxygen inhibition 

and are therefore almost not cured despite the presence 

of light energy for 40 s. Finally, due to reasons of contamination 

and oxygen inhibition, immediate dentin sealing 



or resin coating may be the method of choice to pretreat 

dentin surfaces being chosen for adhesive luting, because 

contamination with temporary cements is avoided and appropriate 

polymerization of the resin-dentin interface is guaranteed. 

12,13,17,21,23,29 This is given even more credence, because 

the present study was able to demonstrate that any 

contamination with temporary cements is crucial, and removal 

methods such as air polishing are sometimes disadvantageous, 

as proven in a previous investigation conducted 

with the effect of air-polishing alone. 2 Finally, both null hypotheses 

had to be rejected. 

CONCLUSIONS 

The dual-cured adhesive provided higher internal bond 

strengths to dentin beneath adhesive inlays. Contamination 

of dentin with temporary cements is a hazard for excellent 

dentin adhesion of adhesive inlays. Therefore, immediate 

dentin sealing is promising. Among temporary cement cleaning 

techniques, polishing air abrasion with Prophypearls severely 

reduces dentin bond strengths. 

REFERENCES 

1. Frankenberger R, Lohbauer U, Schaible BR, Nikolaenko SA, Naumann M. 

Luting of ceramic inlays in vitro: marginal quality of self-etch and etch-andrinse 

adhesives vs. self-etch cements. Dent Mater 2006;submitted. 

2. Frankenberger R, Lohbauer U, Tay FR, Taschner M, Nikolaenko SA. Air-polishing 

powders differently affect dentin bonding. J Adhes Dent 2007; 

accepted for publication. 

3. Frankenberger R, Pashley DH, Reich SM, Lohbauer U, Petschelt A, Tay FR. 

Characterisation of resin-dentine interfaces by compressive cyclic loading. 

Biomaterials 2005;26:2043-2052. 

4. Frankenberger R, Petschelt A, Krämer N. Leucite-reinforced glass ceramic 

inlays and onlays after six years: clinical behavior. Oper Dent 

2000;25:459-465. 

5. Frankenberger R, Sindel J, Krämer N, Petschelt A. Dentin bond strength 

and marginal adaptation: direct composite resins vs ceramic inlays. Oper 

Dent 1999;24:147-155. 

6. Fuzzi M, Rappelli G. Ceramic inlays: clinical assessment and survival rate. 

J Adhes Dent 1999;1:71-79. 

7. Hayashi M, Tsubakimoto Y, Takeshige F, Ebisu S. Analysis of longitudinal 

marginal deterioration of ceramic inlays. Oper Dent 2004;29:386-391. 

8. Hayashi M, Tsuchitani Y, Kawamura Y, Miura M, Takeshige F, Ebisu S. Eightyear 

clinical evaluation of fired ceramic inlays. Oper Dent 2000;25:473- 

481. 

9. Hayashi M, Wilson NH, Yeung CA, Worthington HV. Systematic review of ceramic 

inlays. Clin Oral Investig 2003;7:8-19. 

10. Hayashi M, Yeung CA. Ceramic inlays for restoring posterior teeth. Aust 

Dent J 2004;49:60. 

11. Hikita K, Van MB, De MJ, Ikeda T, Van LK, Maida T, Lambrechts P, Peumans 

M. Bonding effectiveness of adhesive luting agents to enamel and 

dentin. Dent Mater 2006. 

12. Islam MR, Takada T, Weerasinghe DS, Uzzaman MA, Foxton RM, Nikaido T, 

Tagami J. Effect of resin coating on adhesion of composite crown restoration. 

Dent Mater J 2006;25:272-279. 

13. Jayasooriya PR, Pereira PN, Nikaido T, Tagami J. Efficacy of a resin coating 

on bond strengths of resin cement to dentin. J Esthet Restor Dent 

2003;15:105-113. 

14. Krämer N, Ebert J, Petschelt A, Frankenberger R. Ceramic inlays bonded 

with two adhesives after 4 years. Dent Mater 2006;22:13-21. 

15. Krämer N, Frankenberger R. Clinical performance of bonded leucite-reinforced 

glass ceramic inlays and onlays after eight years. Dent Mater 

2005;21:262-271. 

16. Krämer N, Lohbauer U, Frankenberger R. Adhesive luting of indirect 

restorations. Am J Dent 2000;13:60D-76D. 

17. Magne P, Kim TH, Cascione D, Donovan TE. Immediate dentin sealing improves 

bond strength of indirect restorations. J Prosthet Dent 2005; 

94:511-519. 

18. Manhart J, Chen H, Hamm G, Hickel R. Buonocore Memorial Lecture. Review 

of the clinical survival of direct and indirect restorations in posterior 

teeth of the permanent dentition. Oper Dent 2004;29:481-508. 

19. Martin N, Jedynakiewicz NM. Clinical performance of CEREC ceramic inlays: 

a systematic review. Dent Mater 1999;15:54-61. 

20. Mehl A, Kunzelmann KH, Folwaczny M, Hickel R. Stabilization effects of 

CAD/CAM ceramic restorations in extended MOD cavities. J Adhes Dent 

2004;6:239-245. 

21. Nikaido T, Cho E, Nakajima M, Tashiro H, Toba S, Burrow MF, Tagami J. Tensile 

bond strengths of resin cements to bovine dentin using resin coating. 

Am J Dent 2003;16 Spec No:41A-46A. 

22. Nikolaenko SA, Lohbauer U, Roggendorf M, Petschelt A, Dasch W, Frankenberger 

R. Influence of c-factor and layering technique on microtensile bond 

strength to dentin. Dent Mater 2004;20:579-585. 

23. Ozturk N, Aykent F. Dentin bond strengths of two ceramic inlay systems 

after cementation with three different techniques and one bonding system. 

J Prosthet Dent 2003;89:275-281. 

24. Pallesen U, van Dijken JW. An 8-year evaluation of sintered ceramic and 

glass ceramic inlays processed by the Cerec CAD/CAM system. Eur J Oral 

Sci 2000;108:239-246. 

25. Posselt A, Kerschbaum T. Longevity of 2328 chairside Cerec inlays and onlays. 

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26. Reiss B. Clinical results of Cerec inlays in a dental practice over a period of 

18 years. Int J Comput Dent 2006;9:11-22. 

27. Schulz P, Johansson A, Arvidson K. A retrospective study of Mirage ceramic 

inlays over up to 9 years. Int J Prosthodont 2003;16:510-514. 

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preparations: thickness of pre-cured dentin bonding agent and effect of 

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Clinical relevance: Dual-cured adhesives are beneficial 

for adhesive luting. Sealing dentin prior to temporizing 

improves dentin bond strength. 


Sarrett 


XP BOND in Self-curing Mode used for Luting Porcelain 

Restorations. Part A: Microtensile Test 

Ornella Raffaelli a /Maria Crysanti Cagidiaco b /Cecilia Goracci c /Marco Ferrari d 

Purpose: To assess the bond strength to dentin of an experimental adhesive and the proprietary resin cement used 

in different curing modes to lute ceramic disks of different thicknesses. 

Materials and Methods: Empress II disks (Ivoclar-Vivadent) were luted to dentin using XP BOND (Dentsply [XP]) in 

combination with the proprietary self-curing activator (SCA) and cement Calibra (Dentsply [C]). Curing of the adhesive 

was induced either by mixing with the activator (activator, groups 3 to 6) or by light irradiation for 20 s (group 2). The 

cement was either light cured for 40 s through the ceramic onlay (groups 1 to 5) or cured chemically (groups 6 and 7). 

Groups 2 and 4 were compared with group 1, in which Prime & Bond NT (Dentsply DeTrey) was tested as control. In 

groups 3 and 6, 2-mm-thick onlays were luted with XP+SCA, and the cement was light cured for 40 s or let autocure for 

5 min, respectively. These groups were compared with group 7, in which Syntac (Ivoclar Vivadent) was applied with C 

and, in order to reproduce the handling procedures of group 6 (although contrary to manufacturer’s instructions), no 

light irradiation was provided for the adhesive or the cement. The influence of onlay thickness (2, 3, 4 mm) on the 

bond strength developed by XP+SCA/C was assessed by comparing groups 3, 4, 5. In these groups, C was light cured 

for 40 s through the onlay. Microtensile beams were obtained from the luted teeth. 

Results: Bond strengths not including pretest failures (in parentheses: value including pretest failures as 0 MPa) were 

21.0 (17.5) MPa in group 1, 24.9 (21.2) MPa in group 2, 23.7 (21.3) MPa in group 3, 29.9 (26.7) MPa in group 4, 30.3 

(24.6) MPa in group 5, 28.6 (24.6) MPa in group 6, and 17.1 (9.2) MPa in group 7. Statistically significant differences 

were found between groups 1 and 4, groups 3 and 5, and groups 6 and 7. 

Conclusion: The bonding potential of XP BOND used with the activator or light cured in combination with Calibra in 

self- or dual-curing mode outperformed that of a control adhesive-cement system. The bond strength of XP+ SCA + Calibra 

was not negatively affected by the onlay thickness. 


a PhD Student, Department of Dental Materials and Prosthodontics, University of 

Siena, Siena, Italy. 

b Clinical Professor of Dentistry, Department of Dental Materials and Prosthodontics, 

University of Siena, Siena, Italy. 

c Assistant Professor and Chair, Department of Endodontics, University of Siena, 

Siena, Italy. 

d Professor and Chair, Department of Dental Materials and Prosthodontics, University 

of Siena, Siena, Italy. 



Reprint requests: Prof. Marco Ferrari, Research Center for Dental Health, 19 Piazza 

Attias, 57120 Livorno, Italy. Tel: +39-586-892-283, Fax: +39-586-898-305. 

e-mail: ferrarimar@unisi.it 

Many new bonding systems are introduced every year on 

the market. Some of them are primer-adhesive solutions 

in combination with a prior phosphoric acid treatment, 

others avoid the total-etch step and offer self-etching or selfadhesive 

bonding solutions. 3,5,7-10 

However, practitioners would like to use the same bonding 

systems for all clinical applications, although most simplified 

bonding solutions are not necessarily indicated for 

luting indirect restorations, limiting their clinical indications 

to direct restorations. 

Recently, XP BOND (Dentsply DeTrey; Konstanz, Germany), 

using tert-butanol for the first time as solvent in dentistry, 

was proposed as a one-bottle universal adhesive, also 

in combination with a new self-curing activator (SCA). 

When luting a porcelain restoration, differences in thickness 

may reduce the light penetration, resulting in a reduced 

polymerization rate of the luting material. 1,2,4 To avoid 

an incomplete cure of the resin cement adhesive interface, 

the self-curing activator can be used. 

Consequently, the aims of this study were to evaluate (1) 

the procedure for adhesively luting ceramic to dentin and, 

specifically, when light is applied, to cure either the adhesive 

before or after applying the cement, (2) the influence of ceramic 

thickness when the adhesive is not separately light 

cured but mixed with a self-curing activator (SCA), (3) the influence 

of SCA on the bonding efficacy when no light is 

used. The null hypothesis tested is that differences in porcelain 

thickness and curing mode do not affect the bond 

strength values. 


Raffaelli et al 

Table 1 Groups of materials and techniques 

Groups Adhesive Activator Adhesive Cement Ceramic disk 

thickness (mm) 

1 Prime & Bond NT no LC DC 3 

2 XP BOND no LC DC 3 

3 XP BOND yes NC DC 2 



6 XP BOND yes NC CC 2 

7 Syntac* - NC CC 2 

NC: not cured (mix with SCA is applied, but not light cured); LC: light cured (light cured before placement); DC: dual curing (Light is applied on the mixed 

cement); CC: chemically cured (no light is used at all). *According to the directions for use, application and light curing of Heliobond is mandatory when combined 

with self curing materials. 


Bonding was performed on 70 noncarious human third molars 

that were extracted after informed consent had been obtained. 

They were stored in a 1% chloramine T solution at 

4°C and used within one month following extraction. Prior to 

the bonding experiments, the teeth were retrieved from the 

disinfectant solution and stored in distilled water, with four 

changes of the latter within 48 h to remove the disinfectant. 

Tooth Preparation – Bonding to Deep Dentin 

Bonding was performed on the occlusal surfaces of deep 

coronal dentin. The occlusal enamel and the superficial 

dentin of each tooth were removed using a slow-speed saw 

(Isomet, Buehler; Lake Bluff, IL, USA) under water cooling. 

The tooth surfaces were polished with wet 180-grit SiC papers. 

The teeth were divided into 7 experimental groups of 

10 teeth each. The experimental dentin groups are listed in 

Table 1. 

Coupling of Processed Ceramic 

Empress 2 blocks (shade A2) were reduced with the Isomet 

saw under water cooling to produce blocks with dimensions 

similar to those of the teeth to be bonded. Each reduced 

block was then sectioned with the Isomet saw to produce 

2-, 3-, or 4-mm-thick, parallel-sided ceramic onlays. The inner 

surface of each ceramic onlay was sandblasted with 50- 

μm alumina, etched with a hydrofluoric acid gel for 90 s, 

washed, air dried, and silanized using Calibra silane 

(Dentsply). 

To bond the ceramic disks to the dentin surface, the 

bonding systems and the resin cement were used following 

manufacturer’s instructions. As a curing device, a QTH light 

(Dentsply DeTrey) was used (power output: 800 mW/cm 2 ). 

The intensity of the curing light was tested before and after 

curing with a radiometer. The bonded specimens were 

stored in distilled water at 37°C for 24 h before further laboratory 

processing. 

TBS Evaluation and SEM Fractographic Analysis 

Each tooth was sectioned occluso-gingivally into serial slabs 

using an Isomet saw under water cooling. The two slabs from 

each tooth were further sectioned into 0.9 x 0.9 mm ceramic-dentin 

beams, according to the technique for the 

nontrimming version of the microtensile test. 6 Each group 

provided 37 to 53 beams for bond strength evaluation. Premature 

failures that occurred during sectioning were recorded. 

The specimens were stressed to failure under tension using 

a universal testing machine (Model 4440, Instron; Canton, 

MA, USA) at a crosshead speed of 1 mm/min. The data 

were analyzed using one-way ANOVA and Tukey’s multiple 

comparison tests at α = 0.05. 

Representative fractured beams from each of the 7 

groups were air dried and sputter coated with gold/palladium 

for examination with a conventional SEM (Jeol; Tokyo, 

Japan). 

Statistical Analysis 

Three different one-way ANOVAs were performed, each involving 

different groups (Tables 2 to 4). The first two analyses 

were performed in the groups with 3-mm and 2-mm ceramic 

disks, respectively. The last analysis was performed 

on groups with 3 different ceramic thicknesses (2, 3, and 4 

mm) when samples were luted with XP+SCA+Calibra DC. 

Premature failures were excluded from the statistical analysis. 

It was also verified that the tooth of origin was not a significant 

factor for bond strength. 

As the bond strength data were normally distributed (Kolmogorov-Smirnov 

test) and groups had homogeneous variances 

(Levene test), one-way ANOVA was applied to test for 

significance of differences among the tested groups, followed 

by Tukey’s test for post-hoc comparisons. In all the 

analyses, the level of significance was set at α = 95%. 

RESULTS 

The bond strength values found in this investigation are reported 

in Fig 1 and Tables 2 to 4. 



Table 2 Bond strength values obtained luting 3-mm-thick 

porcelain disks. n=sample size (in parentheses, number 

of premature failures), mean, and standard deviation (SD) 

values excluding premature failures. Premature failures 

were excluded from the statistical analysis 

Group N Mean (MPa) SD 

1. (control): 42 (7) 20.9 BC 10 

PBNT LC + 

Calibra DC 

2. XP LC + 53 (8) 24.9 AB 10.7 

Calibra DC 

4. XP + SCA + 37 (4) 29.8 A 12.9 

Calibra DC 

According to the post-hoc test, XP+SCA+Calibra DC achieved a significantly 

higher bond strength than group 1. Groups with the same uppercase 

letter are not statistically significantly different. 

Table 3 Bond strength values obtained luting 2-mm-thick 

porcelain disks. n=sample size (number of premature failures 

in parentheses), mean and standard deviation (SD) 

values excluding premature failures. Premature failures 

were excluded from the statistical analysis 

Group N Mean (MPa) SD 

3. XP+ SCA + 35 (4) 23.6 AB 11.1 

Calibra DC 

6. XP + SCA + 37 (6) 28.6 A 10.4 

Calibra CC 

7. Syntac No LC 20 (17) 17.1 B 6.6 

+ Calibra CC 

According to the post-hoc test, XP+SCA (No LC)+Calibra CC achieved a 

significantly higher bond strength than Syntac No LC+Calibra CC. 

Groups with the same uppercase letter are not statistically significantly 

different. 

Table 4 Bond strength values recorded using 3 different porcelain thicknesses. 

n=sample size (number of premature failures in parentheses), mean and standard 

deviation values excluding premature failures. Premature failures were excluded 

from the statistical analysis 

Ceramic Adhesive/ n Mean (MPa) SD 

thickness resin cement 

Group 3: XP+SCA+Calibra 35 (4) 23.6 B 11.1 

2 mm DC 

Group 4: 

3 mm 33 (4) 29.8 AB 12.1 

Group 5: 

4 mm 43 (10) 30.3 A 12.3 

According to the post-hoc test, the bond strengths measured with 4-mm-thick disks were significantly 

higher than those measured with 2-mm-thick disks. Groups with the same uppercase letter are not statistically 

significantly different. 

Groups 4, 5, and 6 showed the highest bond strength values. 

In these three groups, the XP BOND was not light cured 

before seating the ceramic onlay, and in group 6 Calibra was 

chemically cured. When comparing the groups that differed 

in ceramic onlay thickness, it was noted that the specimens 

obtained from 4-mm-thick onlays (group 5) showed the highest 

bond strength but also a higher percentage of pretest 

failure. 

SEM observations showed that adhesive fracture was 

the most common failure type in groups 2 to 7. Only in group 

1 were two cohesive failures in dentin and two mixed failures 

recorded. 

DISCUSSION 

The microtensile evaluation performed in this study was 

used in order to standardize the bond strength test and evaluate 

two different variables, the restorative material thickness 

and the curing mode of the adhesive-luting agent combinations. 

In order to properly apply the statistical analysis, 

it was decided to report the number of premature failures in 

the tables without including them in the analysis. Only in 

group 7 was the number of premature failures rather high 

(45%). In the other groups, the percentage of premature failures 

was 10% to 19%. The occurrence of premature failures 

may be due to the stress transmitted at the bonding interface 

during the specimen reparation procedure. 



Fig 1 Bond strength values (without 

premature failures) and percentage of 

premature failures (ptf) of the seven 

tested groups. NC: not cured; LC: light 

cured; DC: dual cured; CC: chemically 

cured. 

The results of this study demonstrated that the thickness 

of the porcelain restoration does not affect the polymerization 

of the adhesive/luting combination: in the three groups 

(3 to 5) in which the thickness of porcelain disks was 2, 3, 

and 4 mm, respectively, the bond strength values were between 

23.6 and 30.3 MPa with a progressive increase of 

bond strength proportional to the porcelain thickness. This 

could be due to the efficacy of the self-curing mode of the 

new bonding material and/or to the intrinsically greater 

strength of thicker porcelain. This result should lay to rest 

any doubts that a thick ceramic restoration cannot be luted 

using a one-bottle system in combination with a resin cement. 

The results also suggest that XP BOND can be considered 

a proper bonding system for luting full and partial porcelain 

crowns. In order to simplify the clinical luting procedures and 

according to the results of this study, XP BOND and Calibra 

resin cement can routinely be used in the self-curing mode. 

A study on the clinical performance of XP BOND cured by the 

application of its self-activator and used in combination with 

Calibra resin cement is currently ongoing. 

CONCLUSIONS 

From the results of this study the following conclusions can 

be drawn: 

XP BOND can be used in the self-curing mode in combination 

with SCA and Calibra resin cement for luting porcelain 

restorations. 

The porcelain restoration thickness is not a limitation to 

the curing process of the adhesive-luting material combination 

when XP BOND is self-activated. 



REFERENCES 

1. Bergman MA. The clinical performance of ceramic inlays: a review. Aust Dent 

J 1999;44:157-168. 

2. Davidson CL. Luting cement, the stronghold or the weak link in ceramic 

restorations. Adv Engineer Mater 2001;3:763-767. 

3. De Munck J, Vargas M, Van Landuyt K, Hikita K, Lambrechts P, Van Meerbeek 

B. Bonding of an auto-adhesive luting material to enamel and dentin. Dent 

Mater 2004;20:963-971. 

4. Hahn P, Schaller HG, Hafner P, Hellwig E. Effect of different luting procedures 

on the seating of ceramic inlays. J Oral Rehabil 2000;27:1-8. 

5. Pashley DH, Pashley EL, Carvalho RM, Tay FR. The effects of dentin permeability 

on restorative dentistry. Dent Clin North Am 2002;46:211-245. 

6. Shono Y, Terashita M, Shimada J, Kozono Y, Carvalho RM, Russell CM, Pashley 

DH. Durability of resin-dentin bonds. J Adhes Dent 1999;1:211-218. 

7. Tay FR, Frankenberger R, Krejci I, Bouillaguet S, Pashley DH, Carvalho RM, 

Lai CN. Single-bottle adhesives behave as permeable membranes after polymerization. 

I. In vivo evidence. J Dent 2004;32:611-621. 

8. Tay FR, Pashley DH, Suh BI, Hiraishi N, Yiu CK. Water treeing in simplified 

dentin adhesives - déjà vu Oper Dent 2005;30:561-579. 

9. Tay FR, Pashley DH. Dental adhesives of the future. J Adhes Dent 2002;4:91- 

103. 

10. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M, Vijay P, Van Landuyt 

K, Lambrechts P, Vanherle G. Buonocore memorial lecture. Adhesion to 

enamel and dentin: current status and future challenges. Oper Dent 

2003;28:215-235. 

Clinical relevance: The results of this microtensile investigation 

show good performance of XP BOND in its self-curing 

mode. 


XP BOND in Self-curing mode used for Luting Porcelain 

Restorations. Part B: Placement and 6-month Report 

Marco Ferrari a /Ornella Raffaelli b /Maria Crysanti Cagidiaco c /Simone Grandini d 

Purpose: The aim of this clinical study was to evaluate the postoperative sensitivity of Empress II restorations luted under 

clinical conditions with XP BOND in combination with SCA and Calibra cured in self-curing mode. 

Materials and Methods: Fifty-three restorations were placed in 38 patients in March and April 2006. No patient received 

more than two restorations. Luting procedures were performed following manufacturers’ instructions. The restorations 

were evaluated after 2 weeks and 6 months for postoperative sensitivity, marginal discoloration, marginal integrity, secondary 

caries, maintenance of interproximal contact, and fracture. 

Results: At the 2-week recall, the postoperative sensitivity was reported in only 10 and after 6 months in only 3 patients. 

All other parameters showed alpha scores. 

Conclusion: All the evaluated restorations were in place and acceptable. The postoperative sensitivity recorded after 

using XP BOND and Calibra in self-curing mode was clinically acceptable. 

Keywords: ceramic crowns, self-curing, clinical trial, bonding. 


Indirect ceramic restorations are a valid alternative to direct 

esthetic restorations and to porcelain-fused-to-metal 

crowns. The prerequisite for application of full and/or partial 

porcelain crowns is perfect bonding, which has to integrate 

all parts into one coherent structure. 6 Therefore, luting material 

and technique as well as the substrate characteristics 

represent the factors determining success. 7 

a Dean, Professor, and Chair, Department of Dental Materials and Prosthodontics, 

University of Siena, Siena, Italy. 

b PhD Student, Department of Dental Materials and Prosthodontics, University 


c Assistent Professor, Department of Dental Materials and Prosthodontics, University 


d Chair, Assistent Professor, Department of Endodontics, University of Siena, 

Siena, Italy. 


September 13th, 2006 

Reprint requests: Prof. Marco Ferrari, Research Center for Dental Health, 19 

Piazza Attias, 57120 Livorno, Italy. Tel: +39-586-892-283, Fax: +39-586-898- 

305. e-mail: ferrarimar@unisi.it 

Different combinations of adhesive luting materials have 

been tested, and dual-curing bonding systems are often the 

first choice. 3,5,8,12,14-16,18,19,21 Dual-curing bonding agents 

permit polymerization of the adhesive materials and the 

resin cement underneath a thick ceramic restoration. Recently, 

XP BOND (Dentsply DeTrey; Konstanz, Germany) was 

proposed and tested experimentally, showing interesting data 

when the adhesive was used in self-curing mode. 20 

Postoperative sensitivity is a common complication when 

porcelain crowns are luted on vital teeth. 9 The aim of the present 

prospective clinical trial was to evaluate the early postoperative 

sensitivity of Empress II restorations (Ivoclar-Vivadent; 

Schaan, Liechtenstein), cemented under clinical 

conditions with the adhesive system XP BOND/SCA and Calibra 

resin cement (Dentsply Caulk; Milford, DE, USA), both 

used in self-curing mode. 


The sample consisted of 53 consecutively placed restorations 

in 38 patients in need of one or two single units. Par- 


Ferrari et al 

Table 1 Changes in pre- and postoperative sensitivities (1 = lowest, 10 = highest 

sensitivity) 

case 

XP Bond / SCA / Calibra [n] 

Type of Pre- Postoperative Postoperative 

restoration operative sensitivity sensitivity 

sensitivity (2 weeks (6 months 

after 

after 

placement) 

placement) 

1 Inlay (OD) 0 6 3 

2 Inlay (MOD) 0 1 0 

3 Inlay (MO) 0 1 0 

4 2 onlays 2 0 0 

5 Onlay 0 1 0 

6 Inlay (MOD) 3 1 0 

and onlay 

7 Inlay (MO) 0 1 0 

8 Onlay 4 1 0 

9 Onlay 0 3 2 

10 Inlay (MOD) 0 1 0 

11 Inlay (MOD) 0 3 2 

tial or full restoration was performed from the pool of patients 

accessing the department of Restorative Dentistry of 

the University of Siena. Patients’ written consent to the trial 

was obtained after having provided a complete explanation 

of the aim of the study. 

Inclusion and Exclusion Criteria 

Males and females aged 18 to 60 years in good general and 

periodontal health were included. Patients to whom the following 

factors applied were excluded from the clinical trial: 

1. Under 18 years of age 

2. Pregnancy 

3. Disabilities 

4. Prosthodontic restoration of tooth can be expected 

5. Pulpitic, nonvital, or endodontically treated teeth 

6. (Profound, chronic) periodontitis 

7. Deep defects (< 1 mm from pulp) or pulp capping 

8. Heavy occlusal contacts or history of bruxism 

9. Systemic disease or severe medical complications 

10. History of allergy to methacrylates 

11. Rampant caries 

12. Xerostomia 

13. Lack of compliance 

14. Language barriers 

Test Stimuli and Assessment 

Before applying the adhesive material, a pain measurement 

was performed utilizing a simple pain scale based on the response 

method. Response was determined to a 1-s application 

of air from a dental unit syringe (at 40 to 65 psi at approximately 

20°C), directed perpendicularly to the root surface 

at a distance of 2 cm, and by tactile stimuli with a sharp 

#5 explorer. The patient was asked to rate the perception of 

the sensitivity experienced during this thermal/tactile stimulation 

by placing a mark on a visual analog scale (VAS) beginning 

at 0 and ending at 10 (where 0 = no pain and 10 = 

excruciating pain). In order to translate these scores into 

easily understood pain levels, a score of 0 was defined as 

no pain, 1 to 4 as mild sensitivity (which was provoked by the 

air blast), and 5 to 10 as strong sensitivity (which was spontaneously 

reported by the patient during drinking and eating). 

Only patients scoring low on the VAS were included in 

the study, whereas high score cases were excluded based 

on the assumption that irreversible pulp inflammation could 

be sustaining the high sensitivity. The status of the gingival 

tissues adjacent to the test sites was observed at baseline 

and at each recall. Patients were recalled to our department 

for testing postoperative sensitivity after 2 weeks and 6 

months. 

Clinical Procedure 

For standardization purposes, the same operator performed 

all the clinical procedures. Following anesthesia, the rubberdam 

was placed, all carious structures were excavated, and 

any restorative material was removed. Preparation was performed 

using conventional diamond burs in a high-speed 

handpiece with no bevel on margins. The preparation design 

was dictated by the extent of decay and pre-existing restorations. 

The residual dentin thickness (RDT) was evaluated on 

a periapical radiograph, and teeth with RDT thinner than 0.5 

mm were excluded. After preparation, the impression of the 

prepared tooth was taken and sent to the laboratory. A temporary 

restoration was performed. One week later, the ceramic 

restorations were luted. Luting procedures were performed 

under rubbes-dam. The cavity preparation was 

cleaned with a rotating brush and pumice, and then water 


Ferrari et al 

Table 2 Performance criteria according to Ryge 

Criteria and number of XP Bond 

restorations evaluated after SCA alpha bravo charlie delta 

6 months Calibra[n] 

Marginal discoloration and 53 53 0 0 0 

integrity 

Secondary caries 53 53 0 0 0 

Vitality test 53 53 0 0 0 

Interproximal contacts 53 53 0 0 0 

Retention 53 53 0 0 0 

Fracture 53 53 0 0 0 

sprayed and air dried carefully. 36% phosphoric acid gel was 

then applied for 15 s on enamel margins, and then for other 

15 s on dentin. The gel was removed with air spray and 

the surface blown gently with an air syringe. One drop of XP 

Bond was dispensed and mixed with one drop of self-curing 

activator. Using a microbrush, all cavity walls were wet and 

the adhesive material was left undisturbed for 20 s. After 

that, the solvent was evaporated by thoroughly blowing with 

air from an air syringe for 5 s. No light curing step was performed. 

Calibra Esthetic Resin Cement base and catalyst in 

similar amounts were mixed and applied on the cavity surface. 

Then the restoration was placed in the cavity preparation, 

and resin cement excess was removed with a clean microbrush. 

The Calibra cement was used in self-curing mode. 

The restorations were placed in March and April 2006 and 

examined for postoperative sensitivity at baseline, after 2 

weeks and 6 months by the same operator. At each recall, 

data on postoperative sensitivity, stability, and longevity 

were collected with reference to the USPHS criteria. Therefore, 

the following parameters were assessed: 

• postoperative sensitivity with the restoration under function, 

cold and warm stimuli, and a gentle air stream (on a 

scale from 0 to 10). 

• marginal discoloration and integrity 

• secondary caries 

• fracture 

• vitality test 

• retention 

• interproximal contacts 

The null hypothesis was that the self-curing mode does 

not affect postoperative sensitivity. 

RESULTS 

The results of postoperative sensitivities are summarized in 

Table 1. All 53 teeth were evaluated at baseline, and after 2 

weeks and 6 months. At baseline, 3 patients showed pre-operative 

sensitivity on 5 teeth. Ten cases of postoperative sensitivity 

were observed at the 2-week recall, but only 3 after 

6 months. At the 2-week recall, the postoperative sensitivity 

increased from 0 to 6 in one case immediately after luting 

the restoration (after the anesthetic wore off) but 

dropped to score 3 after 6 months. In 7 cases showing an 

increase in postoperative sensitivity after 2 weeks, the hypersensitivity 

disappeared completely after 6 months. In 

two cases, a residual postoperative sensitivity of score 2 remained 

after 6 months. No adverse events/effects occurred. 

All other parameters showed alpha scores (Table 2). 

DISCUSSION 

Ceramic crowns can be considered a safe type of restoration, 

and are reported to last longer than any other esthetic indirect 

restoration, 15 although many factors influence success, 

such as the kind of ceramic, luting agent, and extension of 

the lesion. Notwithstanding the restoration material, debonding 

and thus microleakage at the gingival margins – particularly 

if located below the cementoenamel junction – cannot 

be completely prevented. 1,8 All these factors are related to 

three subjects: patient, dentist, and material. 11 

In order to control for any additional source of variation besides 

the patient-related variability, one and the same operator 

placed all the restorations in this clinical trial. Inclusion 

and exclusion criteria were followed in order to obtain the 

Ethics Committee’s approval. The occurrence of postopera- 


Ferrari et al 

tive sensitivity was found in around 19% of the restorations, 

with an average score of 1.9. Only in one case of ten was the 

postoperative sensitivity relatively high (score 6), while in 

other cases, the sensitivity was not spontaneous. However, 

at the 6-month recall, the score dropped from 6 (strong) to 

3 (mild). This observation is in agreement with a study that 

reported hypersensitivity to be the most common postoperative 

complication. 17 

The accurate fitting of the crown is another aspect that is 

worth mentioning, even though this property was not explicitly 

assessed in this paper. A good fitting of the ceramic 

restoration can prevent postoperative sensitivity and pulp 

complications. In several studies, it had been reported 12,19 

that the marginal wear of a composite luting cement can undermine 

the mechanical support. To prevent excessive marginal 

wear, it is therefore mandatory to have the narrowest 

possible gap between the cavity preparation and ceramic 

restoration. Optimal fit (ranging from 50 to 100 μm) is preferred, 

8 particularly if the margins extend below the cementoenamel 

junction. 7,9 

A proper adhesive-cement material combination is essential 

for avoiding postoperative sensitivity. Other self-activated 

bonding systems are available on the market and have 

been clinically tested. 5,14 All of them are usually both self-activated 

and light cured in order to guarantee complete polymerization 

of the bonding layer at the surface (where the 

bonding agent can be reached by light) and in deeper areas 

where light cannot penetrate to the adhesive layer. 

The dual-curing resin cements are used in combination 

with the proprietary bonding systems. Accordingly, with the 

limits of this study, the mixture of XP BOND with SCA in combination 

with chemically curing Calibra showed clinically acceptable 

levels of postoperative sensitivity at the 2-week 

and 6-month recalls. These findings will be reevaluated during 

next recalls at 12 months, and 2 and 3 years. 

The utilization of a correct bonding technique is mandatory 

to achieve good clinical results in ceramic inlay luting. 9 

In direct resin restorations, the bonding agent is routinely 

light cured prior to the insertion of the composite. In ceramic 

luting procedures, pre-curing of the adhesive resin may 

make restoration seating more difficult. Also in this regard, 

the use of a self-curing bonding agent is advantageous. In 

the present study, a self-curing cement was chosen for luting 

the restorations. The self-curing cements are able to 

achieve an adequate degree of conversion even at sites 

where light curing may be hindered by the thickness of the 

ceramic. The setting time of the resin cement can also be directly 

correlated to room temperature, glass plate, and 

mouth temperature. 

CONCLUSIONS 

XP BOND used in self-curing mode showed in only one case 

of 53 luted restorations a spontaneous postoperative sensitivity 

of medium intensity after 2 weeks, which dropped to 

a mild grade after 6 months, while all other 9 cases showed 

a very low degree of sensitivity. 



REFERENCES 

1. Alavi AA, Kianimanesh N. Microleakage of direct and indirect composite 

restorations with three dentin bonding agents. Oper Dent 2002;27:19-24. 

2. Bergman MA. The clinical performance of ceramic inlays: a review. Aust 

Dent J 1999;44:157-168. 

3. Dagostin A, Ferrari M. In vivo bonding mechanism of an experimental dual 

cure enamel-dentin bonding system. Am J Dent 2001;14:105-108. 

4. Davidson CL. Luting cement, the stronghold or the weak link in ceramic 

restorations. Adv Engineer Mater 2001;3:763-767. 

5. Fabianelli A, Goracci C, Bertelli E, Davidson CL, Ferrari M. A clinical trial of 

Empress II Porcelain inlays luted to vital teeth with a self-light-curing adesive 

system and a self-curing resin cement. J Adhes Dent 2006;8:427-431. 

6. Ferrari M, Mason PN. Adaptability and microleakage of indirect resin inlays: 

an in vivo investigation. Quintessence Int 1993;24:861-865. 

7. Ferrari M, Mason PN, Fabianelli A, Cagidiaco MC, Kugel G, Davidson CL. Influence 

of tissue characteristics at margins on leakage of class II indirect 

porcelain restorations. Am J Dent 1999;12:134-142. 

8. Ferrari M, Dagostin A, Fabianelli A. Marginal integrity of ceramic inlays 

luted with a self curing resin system. Dent Mater 2003;19:270-276. 

9. Frankenberger R, Krämer N, Petschelt A. Technique sensitivity of dentin 

bonding: effect of application mistakes on bond strength and marginal 

adaptation. Oper Dent 2000;25:324-330. 

10. Hahn P, Schaller HG, Hafner P, Hellwig E. Effect of different luting procedures 

on the seating of ceramic inlays. J Oral Rehabil 2000;27:1-8. 

11. Hickel R, Manhart J. Longevity of dental restorations in posterior teeth and 

reasons for failure. J Adhes Dent 2001;3:45-64. 

12. Krämer N, Frankenberger R, Pelka M, Petschelt A. IPS Empress inlays and 

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mode. 


Sarrett

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