ACID ETCHING

This Library Dissertation is submitted to Sri Ramachandra Dental College and Hospital Sri Ramachandra edical College and Research Institute !Deemed "ni#ersity$ in partial %ul%illment o% the regulation %or the Degree o% aster Dental Surgery in Conser#ati#e Dentistry and Endodontics E&amination held in '(()

Dr*

* SHAN "GARA+

"nder the Guidance o%

,ro%* Dr* S* -alagopal.

*D*S*. *Sc*.

,ro%essor and Head Department o% Conser#ati#e Dentistry and Endodontics Sri Ramachandra Dental College and Hospital ,orur. Chennai / 0(( 110*

CERTI2ICATE
1

This is to certify that the library dissertation entitled 3ACID ETCHING4 here with submitted by Dr* * SHAN "GARA+, in

partial fulfillment for the degree of Master of Dental Surgery in Conservative Dentistry and Endodontics, is a bonafide work carried out by him under my supervision and guidance

Dr* S* -alagopal.
!rofessor and "ead,

*D*S*.

*Sc*.

Department of Conservative Dentistry and Endodontics Sri #amachandra Dental College and "ospital !orur, Chennai $ %&& 11%

'orwarded by

Dr*

*+* Rama5rishnan.

*D*S*.

!rincipal Sri #amachandra Dental College and "ospital !orur, Chennai $ %&& 11%

AC6N78LEDGE ENT
(

) would like to e*press my deepest sense of gratitude to my guide Dr* S* -alagopal. *D*S*. *Sc*. !rofessor and "ead, Department of

Conservative Dentistry and Endodontics, Sri #amachandra Dental College and "ospitals, for his endless hours of enthusiastic involvement, e*pert guidance and his caring support given to me throughout this library dissertation, it has been a remarkable learning e*perience all the way

) Dr*

would

like

to

e*tend

my

heartfelt

gratitude

to

*+* Rama5rishnan.

*D*S*. ,rincipal. Sri #amachandra Dental

College and "ospitals, for permitting me to use the scientific literature and research facilities of the college

My sincere thanks to Dr* Arathi Ganesh.

*D*S*. +ssociate

!rofessor, for her guidance, untiring support and valuable suggestions and for sharing her e*tensive e*perience with me during the entire course

) would be unfair to claim reward individually and not acknowledge the untiring efforts of the team comprising of !rofessors, Dr* ruthyun9aya *D*

S*. Dr* Singara#el ,andiyan. La5shmi -ala9i

*D*S*. and Senior -ecturer Dr* *D*S*. who

*D*S*. -ecturer Dr* ,riscilla Solomon.

supported me at every .uncture

) would also like to give credit to my Co/!0s for their constant support and constructive criticism at every step

My endearing thanks to

r* -as5aran, +nnai 1et !ark, !orur,

Chennai for providing technical support for the study

) would like to thank my ,arents for their constant support and encouragement in pursuing a career in dentistry ) like to thank my beloved :i%e for being a pillar of support during the course, for understanding and bearing me during the different ups and downs of postgraduate life

C7NTENTS
,age no

INTR7D"CTI7N 1 HIST7R; 2 ENA EL 1& 'ormation of enamel 1& Composition of enamel 11 Structure of enamel 1( DENTIN (, !hysical properties (2 Composition of dentin (2 Structure of dentin (2 ACID ETCHING 72 ENA EL 21 Steps in acid etching techni3ue 21 Effects of etching on enamel 24 #ole of fluorides in etching of enamel 25 'actors affecting etching of enamel 4& 6ariation in acid etching methodologies 4( ACID C7NDITI7NING 7% DENTIN 44 0oals of acid conditioning of dentin 4% Effects of acid conditioning of dentin 47 'actors affecting dentin conditioning %7 Conditioners on dentin surface 55 -I7C7 ,ATI-ILIT; 58 <ARI7"S ACID C7NDITI7NERS 7% SEL2 ETCHING ,RI ERS 84 E22ECT 72 ACID ETCHING 7N ,RI AR; TEETH 87 A,,LICATI7NS 72 THE ACID C7NDITI7NERS 1&& 2ACT7RS TA6EN INT7 C7NSIDERATI7N 1&( ACID C7NDITI7NERS 27R GI CE ENTS 1&, -I-LI7GRA,H; 1&4

INTRODUCTION
The possibility of bonding restorative materials to the hard dental tissues intrigued the dental professionals for many years The development and regular use of adhesive materials has begun to revolutioni9e many aspects of restorative and preventive dentistry +ttitudes towards cavity preparation are altering since, with adhesive materials, it is no longer necessary to produce large undercuts in order to retain the filling These techni3ues are therefore responsible for the conservation of large 3uantities of sound tooth structure, which would otherwise be victim of the dental bur

:uonocore ;1844< was the first to report the positive effects of application of 74= phosphoric acid to enamel for the retention of acrylic resin restorations 0winnett, Matsui and :uonocore ;18%8<, further e*plored the effect of acid solutions and this came to be accepted as an integral part of any direct tooth coloured restorative techni3ue

:onding of restorative materials to hard dental tissues would be impossible without the use of acid solutions )t is the effect of these various acid solutions and pretreatments that results in the hard dental tissues being characteri9ed by numerous microscopic porosities, which allows the resin to readily wet the surface and penetrate into these micro porosities >nce the resin penetrates into these micro porosities it can be polymeri9ed to a form a mechanical bond to the hard dental tissues

The success of acid etching of enamel led :uonocore et al ;184%< to try to acid etch dentin using 5= "C- for one minute ?nlike enamel when dentin is etched, surface becomes mineral poor, protein rich, and it tends to become wetter ;:rannstrom and 1orden 6all 1855< ?nfortunately, success with dentin was never reali9ed, because the relatively cured resin materials that were available at that time
%

would not wet dentin very well :uonocore, however, was very much aware of the re3uirements for good bonding The term conditioner or etchant is used to describe agents that are washed off the dentin The word @etchantA has, until recently, been taboo in western dentistry, for describing the action of various acidic materials on dentin Etching of the dentin can be defined as any alteration to the dentin done after the creation of dentin cutting debris, termed the smear layer ;Eick et al 185&<. >ne of the ob.ectives of dentin etching is to create a surface capable of micro/mechanical bonding to a dentin/ bonding agent Several acids have been researched as dentin etchants These include hydrochloric acid, o*alic and pyruvic acid in addition to the better known acid such as phosphoric, maleic, citric and nitric acid and restore with adhesive composite resin +cid etching of dentin is used by many bonding systems to remove the smear layer and permit bonding directly to the dentin matri* +lthough early animal studies indicated that acid etching caused moderate to severe pulpal reactions, there is a high probability that the pulpal irritation may have been due to micro leakage of bacteria and their products +s these reactions are not seen following acid etching of dentin bonding systems 'usayama et al ;1858< were the first to report the successful use of !hosphoric acid to remove the smear layer, etch the dentin

)t is clear that one can acid etch dentin if, and only if, one can seal the dentin with subse3uently placed bonding systems :ecause acid etching increases dentin permeability and dentin wetness, successful bonding of adhesive resins to acid etched dentin re3uires the use of hydrophilic resins that bond e3ually well to both peri tubular and inter tubular dentin The trend seems to be toward lowering both the Bhile all bonding systems concentration of acids and the time of etching of dentin

should be carefully scrutini9ed prior to marketing, the future looks very promising for the use of adhesive resins on both enamel and dentin through the effective use of acid/ etch techni3ue

HISTORY
There are names in the le*icon of dental adhesion that those of us in the field should always remember to acknowledge because it was on their shoulders that we stood as we grappled with our own research problems Dr Michael :uonocore was certainly one of such best/known pioneers in adhesive bonding of resins to teeth "e found that lightly etching enamel created a micro porous surface into which direct filling li3uid resins could flow polymeri9e and make a micro mechanical attachment "e thereby achieved his primary ob.ective of bonding, a conservative means of sealing developmental pits and fissures >ne of Dr :uonocoreCs contemporary Dr
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0eorge 1ewman developed similar methods to bond orthodontic brackets directly to the enamel of teeth +nother distinct advantage of effective acid etching techni3ue and its resultant adhesive bonding to dentin is the prevention of removal of healthy dentin for mechanical retention of composite restorations, a process that is painful without an anesthetics The mechanism of enamel bonding is well understood and involves a micro/ mechanical union between enamel and the resin, which occupies tissue microspores enlarged by the action of an acidic conditioning agent "owever, acid etching of the pulp dentin comple* and its resultant bonding has undergone a number of changes over the last thirty years and both the bond strength values and biocompatibility to pulp dentin organ have tremendously improved

:rannstrom et al ;1872< suggested that on a number of occasions, they inadvertently acid etched teeth with small pulp e*posures at the base of deep cavities These were not often discovered until subse3uent histo/pathological e*amination of the e*tracted teeth ?nless there was concomitant infection there was no particular damage or inflammation to the pulp "owever, they noticed that when restorations leaked, and bacteria coloni9ed the cavity surface, the teeth that had been etched e*hibited more severe pulpal responses, than those that were not etched Many attempts have been made to synthesi9e different coupling agents for tooth surfaces >ne of the earliest successful compounds tested was 1!0/0M+, the reaction product of 1/phenyl/glycine and glycidyl methacrylate ;:owen 18%4< The use of this surface/active co/monomer alone improved the water resistant bonding between resins and enamel and dentin to a degree that was statistically but not clinically significant ;:owen 18%4< #emoval of the structurally weak smeared layer, pellicle, or other superficial layers of the tooth surface by use of acidic ;'usayama D others, 1858, 'usayama 187&< or chelating agents might reduce the availability of calcium ions on dentin
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surfaces for interaction with a chelating surface active co/monomer like 1!0/0M+ or other coupling agent with, preferably, multiple/bonding ligand groups were evaluated for use on tooth surfaces To supplement calcium ion sites for improved bonding, certain appropriate metal cations E*periments indicated that the most effective agent might be ferric o*alate, primarily because of the iron ionCs high tendency to be bound strongly by denting and enamel and its high chelate stability constants with molecules that have linked groups similar to those of 1!0/0M+ ;:owen 1857<

'urthermore, the o*alate would form an insoluble precipitate with calcium ions, which, together with insoluble ferric phosphate, would seal the dental tubules to provide pulp protection and desensiti9ation 1akabayashi ;187(< introduced the concept of hybridi9ation The techni3ue consists of applying an acid, ranging in concentration from 1&= to ,&= to the surface of dentin Bithin 14 minutes the acid selectively dissolves away the inorganic component of the dentin to a depth of 4 to 1& microns )t then flows in to the dentinal tubule for upto 1&& microns at which point it diffuses laterally into the peritubular dentin for up to 1& microns +s in the previous case the calcium component is selectively eliminated Then these spaces are replaced by an insoluble resin component that completely encapsulates all e*posed collagenous fiber )t was then discovered that the additional use of a relatively hydrophilic monomer containing two free carbo*yl groups in addition to two polymeri9able groups on each molecule dramatically improved bond strengths to levels of clinical significance ;:owen and others, 187(< This monomer was called @!MDMA ;the reaction products of pyromellitic dianhydride and hydro*yethyl/methacrylate< There was a synergistic interaction between the 1!0/0M+ and the !MDM ;:owen and others, 1872< The original adhesive system developed was a se3uential application of a3ueous acidic ferric o*alate, followed by an acetone solution of 1!0/0M+ or 1T0/ 0M+ ;the reaction product of 1/ptolyglycine and glycidyl methacrylate<, and then an
1&

acetone solution of !MDM This system was effective only if placed in the described se3uential order utili9ing all three components The acidic ferric o*alate solution was removing the original smear layer, the disturbed surface layer caused by mechanical abrasion in preparing a restoration site ;:owen and others, 1872<, and laying down a layer of precipitation product that was plugging up the lumina of dentinal tubules The latter function significantly reduced tooth sensitivity to the subse3uent procedure The 1T0/0M+ was necessary to induce polymeri9ation of the !MM, but the e*act mechanism of this free radial initiation is still not clear During subse3uent e*perimentation, it was discovered that the smear/ removing capabilities of ferric o*alate were due primarily to the presence of small amounts of nitric acid left over from the synthesis of the o*alate ;Cobb and others, 1878< Controlled additions of nitric acid to the a3ueous o*alate solution were made to determine the optimum acid concentration for this solution ;:losser and :owen, 1877< + small increase in the concentration of nitric acid to about ( 4= "1> , by weight also improved the simultaneous etching of instrumented enamel "owever, an adverse side effect of the application of the ferric o*alate solution was discoveredE the occasional appearance of black staining at the adhesive interface in early animal trails ;Stanley, :owen and Cobb, 1877< This could be reproduced in the laboratory by applying a sodium sulfide solution to ferric o*alate treated dentin The cause of this staining in vivo is probably ;although not proven to be< the reduction of ferric to ferrous ions by sulfide forming anaerobic microorganisms resulting in the formation of black ferrous sulfide pigments To eliminate this, acidic aluminum o*alate was substituted, and it produced no staining on dentin +3ueous solution of aluminum o*alate and nitric acid were then applied, and no staining problems occurred in animal trails ;:losser and others 1878<

There was some evidence in vitro that aluminum o*alate did not produce as much of the reaction products plugging the dentin tubules, as has ferric o*alate Eventually, the first successful transfer of the adhesion technology developed by scientists at the +D+ "ealth 'oundationCs !affenbarger #esearch Center involved the
11

development of a product that incorporated aluminum o*alate in a conditioning solution )n the continuing research, it was found that the aluminum o*alate could be eliminated entirely from the e*perimental system without loss in adhesion, if the dilute nitric acid solution was retained 1one of the other acids evaluated, in a wide range of concentrations, were as good or better than the dilute nitric acid ;which should be distinguished from concentrated nitric acid, a strong o*idi9ing agent< for 1!0/0M+ or 1T0/0M+ three components of Dilute nitric acid 1!0 acetone solution !MDM acetone solution The three components still had to be applied individually in se3uence to adhesive adhesion, and efforts were concentrated on ways to simplify application )t was then suspected and verified that 1!0 would be soluble in the dilute a3ueous nitric acid solution This permitted a simplification of the procedure to the application of two solutions +n acidic 1!0 solution !MDM acetone solution )t was then surprisingly discovered that 1!0 ;1/phenyl/glycine< could be substituted The e*perimental system was then reduced to the

"owever, preparation and storage of the first solution was difficult because of the reactivity of the 1!0 molecule to atmospheric o*ygen Storage times were very short if the acid 1!0 solution was e*posed to air )f the solution was used shortly after mi*ing, adhesion was effective Methods were then developed for preparing the solution under an inert atmosphere and protecting it from subse3uent o*ygen e*posure These protected solutions were solutions were stable under normal storage conditions system Some commercial products are currently based on this two/solution Current e*perimentation with the system is focusing on optimi9ing the
1(

individual components 1itric acid concentrations will continue to be refined to yield optimal treatment of both dentin and enamel Different analogues of the 1!0 molecules are being synthesi9ed toward improving effectiveness, storage, stability and ease of synthesis ;Fohnson, +smussen and :owen 1878< !MDM is being investigated to isolate more effective linking Many years of agents between tooth surfaces and the overlying restorative resins

e*perience in etching enamel with phosphoric acid have shown bonding by this method to be most reliable clinically "owever, it is noteworthy that the use of the chemically functional and more hydrophilic dentin bonding agents, significantly increases bond strengths to acid etched enamel at least in laboratory tests + number of bonding systems already available to practioners are beneficial for increased versatility toward improving the performance of restorative materials +nd, given the high tensile strength of dentin ;:owen and #odrigue9 18%(<, the progress made in the last decade, and the currently recogni9ed need for dentin as well as enamel bonding, it is reasonable to e*pect that before the end of this decade the intensive and e*tensive research efforts will succeed in providing clinicians with completely satisfactory materials and methods for preventive and restorative dentistry by way of adhesive bonding to both dentin and enamel through the reliable use of acid treatments on both enamel and dentin

ENAMEL
Enamel is the most highly calcified and hardest tissue of the body Enamel contains 8%= inorganic portion and 2= organic portion ?nlike dentin, cementum and bone, cells of ectodermal origin )n the human tooth, the enamel normally forms a covering layer for the whole of the crown, but varies considerably in thickness in different parts of the crown ;')0 1< Enamel is a composite material consisting of two phasesG 1G Mineral (G >rganic The mineral phase, an apatite calcium phosphate, is the ma.or component and accounts for the hardness of the tissue The properties of the mineral phase are
1,

modulated dramatically because it is divided into microscopic whiskers or fibers known as crystals The crystals are cemented together by the organic phase, which is a matri* of protein polymer The composite resists brittle fracture far better than does crystalline apatite alone

Formation of Enamel
The long, thin, lathe like crystals that compose enamel are oriented roughly perpendicular to its surface These crystals grow in a gel of protein matri*, which disappears to a large e*tent as the crystals grow within it Eventually, the protein matri* takes the form of e*tremely thin layers, which both glue and separate the enamel crystals The basic orientation of the enamel crystals is perpendicular to the tooth surface

This orientation results from their tendency to grow perpendicularly to the surface on which they develop The developing surface is not simply flat, but is pitted by the secretory poles of the ameloblasts + good three/dimensional picture of the sub/microscopic structure of enamel can be obtained by visuali9ing crystals perpendicular to this peculiarly shaped, pitted surface "owever, it is probably of more significance and greater interest to understand the discontinuities in the enamel structure, which develop at the sharp concavities of the boundaries, or floors and walls, of these pits )t is the arrangement of the crystals at the developing surface that causes the discontinuities in crystal orientation, which we know as the prism boundaries or .unctions These locations ac3uire a more concentrated organic matri* during maturation and in the adult tissue are distinguished by the name @prism sheathsA

Composition of Enamel
The enamel consists mainly inorganic material ;8%=< and only a small amount of organic substance and water ;2=< The inorganic material is apatite The nature of
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the organic constituents of enamel is incompletely understood )n development and histological staining reactions the enamel matri* resembles keratini9ing epidermis More specific methods have revealed sulfydryl groups and other reactions suggestive of keratin ;')0 (< "owever chemical analysis of the matri* of mature enamel indicate that the amino acid composition is not closely related to the keratin and is distinctly different from collagen !roteins can be isolated in several different fractionsE they generally contain high percentages of serine, glutamic acid and glycine #oentgen/ray diffraction studies reveal that the molecular structure is typical of the group of proteins called cross/beta proteins )n addition histochemical reactions have suggested that the enamel/forming cells of developing teeth also contains a polysaccharide/protein comple* and that an acid mucopolysaccharide enters the enamel itself at the time when calcification becomes a prominent feature Tracer studies have indicated that the enamel of erupted teeth of rhesus monkeys can transmit and e*change radioactive isotopes originating from the saliva and the pulp Considerable investigation is still re3uired to determine the normal physiologic characteristics and the age changes that occur in the enamel :rudevold et al ;18%&< reported the inorganic components inorganic components of enamel are principally apatite in its hydro*y, fluoride or carbonate ions Minor variations occur in composition in which aluminium, barium, magnesium, strontium, radium and vanadium among others can be found in the lattice

Structures of Enamel
Enamel rism or Ro! The prism or rod is the fundamental structural unit of enamel, each prism e*tends from its site of origin at the DEF to the outer enamel surface crystals of
14

hydro*yapatite ;')0 ,< +ll enamel with few e*ceptions ;egG very thin enamel< is made up of super assemblies of these structures, combined with varying amounts of interprismatic material Changes in the orientation of the crystals, relative to each other, mark the boundaries of the prisms )n the human enamel, the boundary of the prism body is incomplete cervically "ere the prism is continuous with a wedge/ shaped HtailC, which comparative studies ;:>IDE 18%4< show to be interprismatic enamel The combined shape of the prism body and the tail is that of a keyhole ;')0 2 and 4< The body of the prism is appro*imately 4micron meter wide and the prism plus tail keyhole is appro*imately 8micron meter long ;')0 %< The apatite crystals are most closely packed in the prism bodies, which occupy %&/%4= vJv of enamel ;Shellis 1872< when considered ;')0 5< 'ig 1 Distribution of enamel ;+ Dental enamel covering anatomical crown, : The configuration of enamel crystals is'ig related to the organi9ation of the ( Composition of enamel Dentinoenamel .unction, C Cemento by volume percentage ameloblast enamel and itCs.unction< tomeCs processes The forming surface of enamel consists of pits, each defined by a wall made up of newly formed interprismatic enamel During active secretion, each of these walled pits is occupied is occupied by a tomes processes The inter prismatic walls are formed slightly earlier than the prism enamel, which constitutes the floors of the pits and are formed by secretion sites at the ameloblasts peripheries The presumptive prism boundary is defined by the position of the .unction 'ig 2 >rientation of between pit wall and the floor )n human enamel the pit is at itCs deepest crystals in forming 'igthe , )ndividual enamel rod head D tail rods and inter digiti9ing with confluent with the wall cervically, occlusally, rises to become thus eliminating the neighboring rods boundary in this region Each wall ;inter prismatic region< is formed as a cooperative effort by ad.acent secretory ameloblasts :ased on current knowledge of enamel formation, it is clear that each ameloblast is responsible for the formation of one prism at its central secretary site and a portion of the surrounding inter prismatic region at its cooperative peripheral sites thus cannot be packed as tightly together )nter prismatic enamel contains more enamel protein than the prism bodies, because the crystals meet at different angles and

1%

'ig 4 >rientation of enamel rods

The consistent arrangement of the inter prismatic enamel, with its greater protein content, accounts for the fish scale appearance observed in ground sections
15

Due to its ultra/structural organi9ation, enamel despite itCs hardness and density/ has appreciable porosity The pore affects the mechanical and optical properties of enamelE the formation of carious lesions is strongly influenced by the pathways for diffusion and by electro chemical effects arising from the charge on the pore wall The prism .unctions or boundaries, which are the sites where crystals of the tail region of one prism meet with those in the body of another, are sites where there is an abrupt change in the crystal orientation Conse3uently, prism .unctions have enlarged pores, filled with matri* and hence increased porosity ;"amilton et al 185,< )n human enamel the incomplete prism .unctions form laminar pores with curved cross/section running from the dentinoenamel .unction to the outer surface )n outer enamel the prism .unctions tend to separate, and thus e*ist as independent channels, whilst those in inner enamel ;especially in molars< interconnect to form a three/dimensional network of laminar spores ;:oyde 1878, Shellis 188%< Enamel mineral is composed of relatively small crystals, the arrangement of which results in internal pores that are small and variable in form, orientation and distribution Chromium soleplate deminerali9ation has been used to provide ultra structural information on the distribution of matri* ;Sundstrom and Kelander 18%7< used this techni3ue, and reported individual crystals with a coating of matri* Matri* is more apparent in the tail region than in the body region The material at prism .unctions has a raised solubility ;Shellis 188%<, which may be due to the deposition of the mineral with increased magnesium and carbonate content during amelogenesis, leading to the formation of sites with defective, more soluble apatite ;Shellis 188%< The increased solubility at the prism .unctions, combined with faster diffusion in this region, accounts for the deminerali9ation pattern observed in advancing carious lesions +t such lesions sites deminerali9ation occurs preferentially via these prism .unctions and then spreads laterally into the inter prismatic regions Bhile the largest pores in enamel are associated with the prism .unctions, they only contribute in a small way to the total porosity, most of which is associated with prism bodies and
17

tails "ere, the pores e*ist as very narrow gaps between closely packed crystals but some, while small, are elongated and tubule like and may communicate with the prism .unction pores only through narrow inter crystalline pores Enamel rods follow a wavy, spiraling course, producing an alternating arrangement for each group or layer of rods as they change direction in progressing from the dentin toward the enamel surface where they end a few micrometers short of tooth surface ;')0 7< Enamel rods rarely run a straight radial course because it appears there is an alternating clockwise and counterclockwise deviation of the rods from the radial course at all levels of the crown They initially follow a curving path through one third of the enamel ne*t to the dentino/enamel .unction +fter that, the rods usually follow a more direct path through the remaining two thirds of the enamel to the enamel surface :oyde ;185%< stated that the keyholes shape of the prisms in cross section tends to prevent slip across prism boundaries under lateral shear development surface by ameloblast "narle! Enamel There are groups of enamel rods that may entwine with ad.acent groups of rods, and they follow a curving irregular path towards the tooth surface These comprise gnarled enamel, which occurs near the cervical regions and the incisal and occlusal areas ;')0 4< 0narled enamel is not sub.ect to cleavage as is regular enamel This type of enamel formation does not yield readily to pressure of bladed, hand cutting instruments in tooth preparation ;')0 8< Hunter Sc#re$er %an!s The changes in the direction of the enamel prisms that minimi9e cleavage in the a*ial direction produce an optical appearance called "unter Schreger bands ;')0 1& and 11< These bands appear to be composed of alternate light and dark 9ones of varying widths that are slightly different permeability and organic content These bands are found in different areas of each class of teeth Since the enamel rod orientation varies in each tooth, "unter $ Schreger bands also have a variation in the
18

The keyhole

configuration results from the uni3ue shape of the typical pit produced on the

number present in each tooth )n the anterior they are located near the incisal surface They increase in the number and areas of the teeth from, the canines to the premolars in the molars the bands occur from near the cervical region to the cusp tips The orientation of the enamel rod heads and tails and gnarling of the enamel rods provide strength by resisting, distributing, and dissipating impact forces )n the inner one/half to two thirds of the enamel, curvature of the prisms is responsible for the formation of "?1TE#/SC"#E0E# :+1DS Each band consists of 1&/1, prisms, which in alternate bands are sectioned appro*imately longitudinally or appro*imately transversely "owever the transition between alternate bands is gradual

'ig % Ley hole shaped enamel rods

'ig 5 Enamel rods in cross section

'ig 7 Enamel rods appear wavy in section of enamel

'ig 8 0narled enamel

(&

'ig 1& !hotomicrograph of enamel illustrating phenomenon of light D dark bands ;"unter Shregar :ands<

'ig 11 "unter $ Shregar :ands when enamel is viewed under polari9ed light

Enamel Tufts Enamel tufts are hypo/minerali9ed structures of enamel rods and inter/rod substance that pro.ect between ad.acent groups of enamel rods from the dentino/ enamel .unction ;')0 1( and 1,< these pro.ections arise in the dentin, e*tend into the enamel in the direction of the long a*is of the crown, and may play a role in the spread of dental caries ;>rams et al 185%< Enamel Lamellae They are thin leaf faults between enamel rod groups that e*tend from the enamel surface towards the dentino/enamel .unction, sometimes e*tending into the dentin ;')0 1(< They contain mostly organic material, which is a weak area predisposing a tooth to the entry of bacteria and dental caries ;')0 12< Enamel Spin!les >dontoblastic processes sometimes cross the dentino/enamel .unction into the enamelE these are termed enamel spindles when their ends are thickened ;')0 1(< They may serve as pain receptors, there by e*plaining the enamel sensitivity e*perienced by some patients during tooth preparation ;')0 14<
(1

These regions are of high porosity, as they cut across the

prism structure, in which crystals are small and dispersed and protein abundant

Incremental Lines of Enamel & Striae of Ret'ius Enamel rods are formed linearly by successive opposition of enamel in discrete increments ;')0 1%< The resulting variations in structure and minerali9ation are called the )ncremental Striae of ret9ius and can be considered growth rings ;')0 1(<

'ig 1( !hotomicrograph e*hibiting enamel tuft, enamel lamellae, enamel spindle, striae of ret9ius, Dentino enamel .unction

'ig 1, Transmitted light micrograph of DE .unction showing enamel tufts

((

'ig 14 Enamel spindles

'ig 12 Enamel lamellae

)n hori9ontal sections if the tooth, the Striae of #et9ius appear as concentric circles )n vertical sections, the lines transverse the cuspal and incisal areas in a symmetric arc pattern descending obli3uely to the cervical region and terminating at the dentino/enamel .unction Bhen these circles are incomplete at the enamel surface, a series of alternating grooves, called the imbrication lines of !ickerill, are formed The elevations between the groves are called !erikymataE these are continuous around the tooth and usually lie parallel to the cemento/enamel .unction and each other The enamel of deciduous teeth develops partly before and partly after birth The boundary between the two portions of enamel in the deciduous tooth is marked by an accentuated incremental line of ret9ius, the neonatal line or neonatal ring ;')0 15< )t appears to be the result of abrupt change in the environment and nutrition of the newborn infant enamel The prenatal line is usually well developed than the postnatal This is e*plained by the fact that the foetus develops in a well/protected

environment with an ade3uate supply of all the essential materials, even at the e*pense of the mother )n addition, it has been reported that there is locally increased porosity at the incremental growth lines ;1ewman and !oole 1852< +s a result, enamel structure is altered along these lines and electron microscopy has reveled a possible decrease in the number of crystals in the striae There is also increased porosity on the cross striations ;:oyde 1878<, which are a pattern of periodic banding noted at (/% micron meter intervals along the length of the prisms, and which represent the circadian variation in secretory activity of the ameloblast Shellis ;188%< produced methacrylate replicas of some cross striations in inner enamel, but was unable to do so in outer enamel, suggesting that the pores at most striations are very small or inaccessible )n cuspal enamel the prism curvature gives rise to a related but often apparently more complicated appearance of gnarled enamel :ands in which the prisms run
(,

parallel with the section plane reflect the light to a different degree compared with those in which the prisms are perpendicular to the section plane ;Silverstone 187(< :ecause of the deviations in prism orientation, inner enamel is relatively porous )t is thought that the relatively complicated prism arrangement within the "unter/Schreger bands to reduce the propagation of fractures ;>sborn 18%7, :oyde 1878< )n the outer enamel, the prisms are straight and parallel in the cuspal and lateral regionsE so do not show "unter/Shreger banding The angle at which prisms reach the surface varies with the anatomical location on the tooth +t the cervical margin, the prisms follow an undulating course and approach the surface at very variable times acute angles ;:oyde 1878< >cclusally different orientation is noted, with prisms on the lateral surface of the crown being angled at appro*imately 5& , whilst on the cuspal surface the angle returns to appro*imately 8& rism S#ape an! Cr(stal Orientation The cross sectional appearance of prisms is by the inter/relationship of prismatic and inters prismatic enamel ;')0 17< Three classical prism patterns have been defined, termed ;)&*< ;:oyde 1878< attern ) )s characteri9ed by prisms with complete boundaries, separated by well defined inter prismatic regions

attern + The prisms have incomplete outlines and are arranged in rows Bithin each rows narrow bridges of inter prismatic enamel separate the rows attern * )s the structure observed in human enamel, containing alternating prisms with horseshoe shaped boundaries
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+lthough pattern , is predominant in human enamel ;:oyde 1878<, the other patterns can be found in restricted areas )n particular, pattern 1 enamel, occurs close to the dentinoenamel .unction and also near the outer surface i e , in the enamel formed at the beginning and end of the ameloblast life cycle Comparative studies show that there is no correlation between prism pattern and incremental rate )n all the three patterns, crystals in the inter prismatic regions are oriented appro*imately perpendicular to the general forming surface ;i e , perpendicular to the plane of the ret9ius lines<, while the crystals within the prisms form perpendicular to the floor of the TomeCs process pit )n human enamel, this results in a gradual divergence of the crystals in the tail region from the parallel intra prismatic arrangement by angles of about 14 /24 in the cervical direction ;!oole and :rookes 18%1< )n pattern ( enamel it results in a large angle between the interprismatic crystals and those in the prism sheets This distinction between pattern ( and pattern , is important because of the widespread use of rodent and bovine enamel ;pattern (< in dental research

Cr(stal Si'e an! Morp#olo$( The crystals of mature enamel appear to grow and fill the bulk of the space available within the prism The apatite crystals characteristically e*hibit considerable irregularity of outline, but are roughly he*agonal in cross/section, with a mean width of %7 , nm and mean thickness of (% ,nm Many of the crystals in mature enamel show evidence of crystallographic defects ;)chi.o et al 188,< Aprismatic Enamel +prismatic enamel, up to 1&&/micron meter thick, has been reported to be present at the surface of both permanent and deciduous human enamel ;:oyde 1878, Lodaka et al 1878< ;')0 18< The thickness of aprismatic enamel varies both within
(4

and between tooth types Bithin aprismatic surface enamel, the crystals are arranged parallel to each other and perpendicular to the surface, although some deviation in crystal orientation, due to the presence of remnants of prism boundaries, may be detectable in some areas ;Lodaka et al 1878< :ecause of the parallel alignment of crystals and the absence of prism boundaries, the surface layer is generally more highly minerali9ed than the subsurface enamel ;#obinson et al 1851< This relatively featureless layer is thought to be result from the loss of the tomes Hprocess by the ameloblastE thus the structural feature which directs the deposition of crystal into prisms and interprismatic material is lost, altering enamel structure as a conse3uence

Dentino Enamel ,unction The interface of the enamel and dentin is called the dentinoenamel .unction ;')0 1(< )t is scalloped or wavy in outline, with the crest of waves penetrating toward the enamel The rounded pro.ections of the enamel fit into the shallow depressions of the dentin This inter digitations seems to contribute to affirm attachment between dentin and enamel The dentino/enamel .unction is also a hypo/ minerali9ed 9one about ,& micrometer thick ;')0 (&< Enamel is incapable of repairing itself once destroyed because the ameloblast cell degenerates following formation of the enamel rod The final act of the ameloblast cell is secretion of a membrane covering the end of the enamel rod This layer is referred to as 1asmyth membrane, or the primary enamel cuticle This membrane covers the newly erupted tooth and is worn away by mastication and cleaning The membrane is replaced by an organic deposit called a pellicle, which is a precipitate of salivary proteins Microorganisms may invade the pellicle to form bacterial pla3ue, a potential precursor to dental disease
(%

(5

'ig 1% 0round section of enamel viewed under transmitted light showing striae of ret9ius

'ig 15 !hotomicrograph showing prenatal and post natal enamel in primary teeth

'ig 17 Different prism patterns in transverse section

'ig 18 +prismatic enamel

DENTIN

'ig (& The Scalloped appearance of dentino enamel .unction

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Dentin provides the bulk and general form of the tooth and is characteri9ed as a hard tissue with tubules throughout the thickness )t forms slightly before the enamelE it determines the shape of the crown, including the cusps and ridges and the number and si9e of the roots ;')0 (1< +long the crown, the dentin is covered by enamel, along the root by cementum )t encloses the dental pulp, with which it shares a common origin from the dental papilla The dentin and pulp can be considered as a single development and functional unit, often described as pulpodentinal comple* Dentin can be defined as porous biological composite composed of apatite crystal filler particles in a collagen matri* ;!ashley 188%< The apatite crystallites are thought to provide strength, where as the collagen matri* provides toughness Dentin contains dentinal tubules surrounded by highly minerali9ed ;84= volume mineral phase< intratubular dentin embedded within a partially minerali9ed ;,&= volume mineral phase< collagen matri* ;inter tubular dentin< ;Marshall et al 1885< The ma.ority of tooth structure is composed of dentin, which is the vital component of the tooth Bhen compared with the enamel ;Lnoop hardness number L"1 ,2,<, dentin is much softer ;L"1 %7< ;Craig 188,<, a characteristic e*plains why dentin e*hibits much faster wear )n addition the modulus of elasticity of enamel is appro*imately 72 0pa ;Craig 188,< compared with a value of 1,/15 0pa reported for dentin

#(sical roperties
)t is light yellow in colour and becomes darker with age and less translucent )t is harder than bone and cementum but softer and less brittle than enamel Dentin has greater compressive strength and tensile strength than enamel because it is traversed by tubules The dentin is readily permeable Specific gravity $ ( 1gJml Dentin is elastic and sub.ect to slight deformation and acts as a shock absorber to overlying
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enamel The lower mineral salt content in dentin renders it more radiolucent than enamel Compressive strength of dentin / 2& $ 4&,&&& !S) Modules of resilience vital dentin $ 1&&/12& -:SJ)nch Modules of vital dentin $ 1,8&,&&& psi

Composition of Dentin
5&= / )n organic material (&= / >rganic Materials 1&= / Bater The inorganic substance consists of hydro*yapatite crystals and small amount of phosphate, carbonates and sulfates ;')0 (,< The organic substance consists of type/1, collagen containing (&= of matri* with proteoglycans between the fibres

Structure of Dentin
Dentinal Tu-ules The dentinal matri* contains tubules, each or which ranges from about 1 to (micro meter in diameter at its outer end and , to 2micrometer at is pulpal side The number of tubules are about 14,&&& Jmm ( near the dentinoenamel .unction and it is %4,&&&mm( near the pulpal surface The dentinal tubules are fine canals that e*tend across entire width dentin They contain odontoblastic process curvature and secondary curvatures ;')0 ((< !rimary curvature start at right angle from the pulpal surface, the conve*ity of this curved course is directed towards the ape* of the root and the curvature in the outer half is directed towards the occlusal or incisal surface These tubules end perpendicular to the dentino/enamel .unction and cemento/dentinal .unction )t is almost straight at the root ape*, incisal edges and cusps >ver their entire, length, the tubules e*hibit minute relatively regular secondary curvatures ;')0 (2< of the The course of the dentinal tubules

follows a gentle curve, which is @SA Shaped They show two curvatures / primary

,&

The fore most morphological characteristic of dentin is itCs tubular branched structure the pulp to the dentino/enamel .unction ?nder normal conditions the tubules are filled with fluid, may be important in hydraulically transferring and relieving stresses imparted to dentin through the supporting structures of the periodontium and the enamel )ndeed this may e*plain why endodontically treated teeth are more brittle than vital teeth Bhen isolated from the dentin, each individual dentinal tubule would have the appearance of an inverted coneE with the smallest dimension being recorded at the dentino/enamel .unction end the largest dimension ad.acent to the cell body in the pulp Canaliculi or Microtu-ules The dentinal tubules have lateral branches throughout the dentin termed as canaliculi These canaliculi are1micrometer or less in diameter and originate more or less at right angle to the main tubule

'ig (1 Structures seen in dentin

'ig (( S/shaped dentinal tubules

'ig (, Composition of dentin by volume percentage

,1

'ig (2 Dentinal tubules seen in longitudinal ground section showing primary and secondary curvatures

Enamel Spin!les 1ear the dentino/enamel .unction, the dentinal tubules divide into several terminal and form an inter communicating and anastomosing network Some dentinal tubules e*tend into the enamel for several millimeters These are formed as enamel spindles ;')0 14< eritu-ular Dentin The dentin that immediately surrounds the dentinal tubules is called peritubular dentin This dentin forms the walls of the tubules )t is more highly minerali9ed about 8= than the intertubular dentin )t is completely broken down and disappears on being sub.ected to routine decalcification methods Intertu-ular !entin The main body of the dentin is composed of intertubular dentin )t is located between the dentinal tubules or between the 9ones of peritubular dentin +lthough it is highly minerali9ed this matri*, like bone and cementum is retained after decalcification +bout one half of its volume is organic matri*, specially collagen
,(

fibres which are randomly oriented around the dentinal tubules The fibres have a lattice like arrangement coursing in gentle curves between the tubules and their peri/ tubular 9ones The fibres also e*hibit cross/bonding "ydro*yapatite crystals are formed along the fibres Bithin each tubule is a collagen/deficient, hyper minerali9ed layer of dentin, which has been termed as peritubular dentin, and which may be more accurately termed periluminal ;!ashley 188%< or intratubular dentin, which is calcium deficient carbonate rich hydro*yapatite The small crystals present have a higher crystallinity and are five times harder than the intertubular dentin, with L"1 of (4& compared with a L"1 of 4( for intertubular dentin The presence of this intertubular dentin narrows the lumen of the tubule from its original ,/m to as little as & %/ & 7 m in superficial dentin near the dentino/enamel .unction The width of intratubular dentin decreases in a pulpward direction, where there is a 9one in which there is no intratubular dentin present and the tubule ;luminal< diameter is appro*imately ,m ;0arberoglio and :rannstrom 185%< There is little published information on the biological control of intra tubular apposition, but it is known to be a slow process, slower than the incremental formation of secondary dentin in the pulp chamber re !entin !redentin is located ad.acent to the pulpal tissue and is ( m to %m wide )t is the first formed dentin and is not minerali9ed +s the collagen fibres undergo minerali9ation at the pre/dentin front, the predentin then becomes dentin and a new layer of predentin forms circumpulpally ;')0 (4< O!onto-lasts The cells, which are related to the deposition of dentin, are the odontoblasts The odontoblasts are a layer of speciali9ed cells, which lie on the surface of the pulp
,,

against the internal surface of the dentin )n a fully formed tooth, the odontoblasts are arranged at a single layer of closely packed cells, which are pyriform, in shape +s the cells are the cells are at different levels in the layer, on erroneous impression of stratification results Each odontoblast possesses a long process ;TomeCs 'ibres<, which passes from the distal end of the cell into the substance of the dentin where it is housed in a fine canal, the dentinal tubules The odontoblastic processes are largest in diameter near the pulp ;, to 2m< and taper upto 1mm further into dentin ;')0 (%, (5 and (7< rimar( Dentin The dentin that forms the initial shape of the tooth is called primary dentin )t is usually completed three years after tooth eruption circumpulpal dentin ;')0 (8< Mantle Dentin Mantle dentin is the name of the first formed dentin in the crown underlying the dentino/enamel .unction )t is thus the outer ;or< most peripheral part of the primary dentin and it is about (&Mm thick The fibrils formed in this 9one are perpendicular to the dentino/enamel .unction and the organic matri* is composed of the collagen fibrils ;')0 ,&< Circumpulpal Dentin Circumpulpal dentin forms the remaining primary dentin or bulk of the tooth )t is circumpulpal dentin that represents all of the dentin formed prior to root completion The fibrils in circumpulpal dentin are much smaller in diameter and are more closely packed together The circumpulpal dentin may contain slightly more mineral than mantle dentin )t consists of mantle and

,2

'ig (4 !redentine

'ig (% >dontogenic 9one comprising odontoblasts, cell rich 9one, cell free 9one

'ig (7 E*tension of odontoblast process in dentinal tubule

'ig (5 SEM of deep dentin showing odontoblastic process

'ig (8 !rimary dentin and secondary dentin

Secon!ar( Dentin

'ig ,& "istology of mantle dentin

,4

Secondary dentin is a continuation of primary dentin that forms at a slower rate as the tooth ages physiologically )t is a narrow band of dentin bordering the pulp and represents the dentin formed after the root completion Secondary dentin formation takes place without any e*ternal stimuli )n secondary dentin, the tubules take a different directional pattern in contrast to primary dentin ;')0 (8< Incremental Lines The incremental lines von ebner or imbrication lines appear as fine lines ;or< striations in dentin ;')0 ,1< They run at right angles to the dentinal tubules and correspond to the incremental lines in enamel ;or< bone These lines reflect the daily rhythmic, recurrent deposition of dentin matri* as well as hesitation in the daily formative process The distance between lines varies form 2 to 7Mm )n the crown to much less in the root The course of the lines indicates the growth pattern of the dentin Contour lines of O.en >ccasionally some of the incremental lines are accentuated because of the disturbances in the matri* and minerali9ation process Such lines are readily demonstrated in ground sections and are known as contour lines The most consistently seen contour lines is at the .unction of the primary and secondary dentin ;')0 ,(< Neonatal Lines )n the deciduous teeth and in the first permanent molars, where dentin is formed partly before and partly after birth, the prenatal and postnatal are separated by an accentuated contour line This is termed as neonatal line and is seen in enamel and as well as dentin This line reflects the abrupt change in the environment that occurs at birth The dentin matri* formed prior to birth is usually of better 3uality than that formed after birth and neonatal line may be a 9one of hypo/calcification ;')0 ,,<
,%

Inter "lo-ular Dentin Some times minerali9ation of dentin begins in small globular areas that fail to fuse into a homogenous mass This results in 9one of hypo/minerali9ation between the globules These 9ones are known as interglobular dentin )nter globular dentin forms in the crown of teeth in the circumpulpal dentin .ust below the mantle dentin, and it follows the incremental pattern ;')0 ,2< The dentinal tubules pass un/interruptedly through interglobular dentin, thus demonstrating defects of minerali9ation and not of matri* formation )n dry ground sections some of the interglobular dentin black in transmitted light "owever, spaces in interglobular dentin are not believed to occur naturally 'ig ,1 6on EbnerCs lines 'ig ,( Contour lines of >wen "ranular La(er Bhen dry ground section of the root dentin is visuali9ed in transmitted light, there is a 9one ad.acent to the cementum that appears granular This is known as tomes ;or< granular layer ;')0 ,4< This 9one increases slightly in amount from the Cementoenamel .unction to the root ape* and is believed to be caused by a coalescing and looping of the terminal portions of the dentinal tubules The cause of development of this 9one is probably similar to the branching and beveling of the tubules at the dentinoenamel .unctions 'ig ,, 1eonatal line in dentin

'ig ,2 0round section of dentin viewed under transmitted light showing interglobular dentin

,5

'ig ,4 0round section of dentin, viewed under polari9ed light showing granular layer

A"E AND FUNCTIONAL CHAN"ES Reparati/e Dentin #eparative dentin is formed by the replacement ;or< secondary odontoblast in response to irritation caused by attrition, abrasion, erosion, trauma, dental caries, some operative procedures and other irritants ;')0 ,% and ,5< #eparative dentin is formed when Tomes !rocess are cut within 1 4 mm from the pulp The cut fibres die along with the corresponding odontoblasts leaving dead tracts 1ew odontoblasts are
,7

differentiated from mesenchymal cells of the pulp in about 14 days and these replacement odontoblasts lay down the reparative dentin Dea! Tracts This is a type of reaction dentin, which appears to result from irritation of greater severity The odontoblast process in the whole length of the in.ured tubule degenerates and at the same time is sealed off at the pulpal end by a deposit of reactionary dentin ;')0 ,7< )n dried ground section of normal dentin the odontoblast processes disintegrate and the empty tubules are filled with air They appear black in transmitted and white in reflected light -oss of odontoblast process may also occur in teeth containing vital pulp as a result of caries, attrition, abrasion, cavity preparation ;or< erosion, ;Bhen the tomes process are cut more than 1 4mm< These areas demonstrate decreased sensitivity and appear to a greater e*tent in older teeth

Sclerotic Dentin Sclerotic dentin results from aging or mild irritation ;such as slowly advancing caries< and causes a change in the composition of the primary dentin The peritubular dentin becomes wider, gradually filling the tubules with calcified material, progressing from the D E Function pulpally These areas are harder, denser, less sensitive, and more protective of the pulp against subse3uent irritations ;')0 ,8< The deposition of intratubular dentin, as a result of ageing or in response to attrition, results in a progressive reduction in the tubule lumen, and if continued, obliterates the tubule )f this occurs in several tubules in ad.acent areas, the dentin assumes a glassy appearance The term used to describe this progressive deposition and obliteration of the tubule is SC-E#>S)S, resulting in sclerotic dentin This process begins in root dentin of 17 $ year old premolars without any e*ternal influence )t can therefore be assumed that this is a physiological response
,8

and the occlusion of the tubules is achieved by continued intratubular deposition The mechanism by which intratubular dentin is formed are poorly understood and three possible mechanisms have been suggested ;Torneck 1882< Firstly, it has been suggested that there may be a passive redistribution of mineral from inter tubular dentin into the tubules around the pre/e*isting components of the tubule Secondly there may be an active response on the part of the odontoblast process, resulting in an organic matri* that is actively minerali9ed as a result of odontoblast activity Finally, it has been suggested that the odontoblast may produce an organic matri* that becomes minerali9ed by redistribution of mineral from 'ig ,% #eparative dentin intertubular dentin, as in the first case )n which ever way it is formed, the net result is that intratubular dentin is deposited at the e*pense of the odontoblast process, which is either retracted or shortened by the loss of itCs distal e*tremity

'ig ,5 Types of reparative dentin

2&

'ig ,7 Dead tracts / ground section of dentin viewed under transmitted light

'ig ,8 Sclerotic dentin

The amount of sclerosed dentin increases with age and is most fre3uently encountered in the apical third of the root Sclerosis reduces the permeability of dentin and thus may help prolong pulp vitality !rocesses, which contribute to sclerotic dentin in the crown in response to attrition and caries, may differ from the physiological deposition of sclerotic ;translucent< dentin in the root, which is age/dependent and whose rate of deposition is not altered by attrition +lthough there is a little evidence in the literature, it is thought sclerosis resulting from aging is physiological dentin sclerosis and that resulting from mild irritation is reactive dentin sclerosis Eburnating dentin is a term referring to the outward portion of reactive sclerotic dentin where slow caries has destroyed formerly overlying tooth structure, leaving, a hard, darkened, cleanable surface The refractive indices of dentin in which the tubules are occluded are e3uali9ed and such areas become transparent Transparent ;or< sclerotic dentin can be observed in the teeth of the elderly people, especially in the roots Sclerotic dentin may also be found under slowly progressing caries Mineral density is greater in this area of dentin as shown both by radiography and permeability studies )t appears transparent or light in transmitted light and dark in reflected light
21

INNER0ATIONS OF DENTIN Intertu-ular ner/es Dentinal tubules contain numerous nerve endings in the predentin and inner dentin no further than 1&& to 14&Mm from the pulp Most of these small vesiculates endings are located in the tubules in the coronal 9one, specifically in the pulp horns The nerves and their terminals are found in close association with the odontoblast process within the tubule ;')0 (7< 1erve grows into the papilla in the bell stage of tooth development ;:yers 187&< both afferent neurons and efferent automatic nerves that innervate pulpal blood vessels are present The number of myelinated a*ons in permanent teeth increases with age and Jor tooth development, reaching a plateau value of about 4&& myelinated a*ons per human premolar at age 14, which remains constant upto %& years There may be single terminals or several dilated and constricted portion )n either case, the nerve endings are packed with small vesicles, either electron dense or lucent, which probably depends on whether there as been discharge of their neuro transmitter substance )n any case, they interdigitate with the odontoblast process, indicating an intimate relationship to this cell )t is believed that most of these are terminal processes of the myelinated nerve fibres of the dental pulp The primary afferent somato sensory nerves of the dentin and pulp pro.ect to the main sensory nucleolus of the midbrain E1tent of O!onto-lastic rocess

During tooth development, at the bell stage, odontoblast processes e*tend from the odontoblast cell body through predentin to the dentino/enamel .unction +s the thickness of dentin increases, the cellular processes must elongate
2(

"owever, the true length of the processes in mature dentin, in the absence of blood vessels or supporting cells, is an issue that is open to debate ;')0 (7< )n human teeth, the thickness of dentin is about ,/, 4mm Such that if an odontoblastic process were to pass the entire distance from the pulpal border to the DEF, then the volume of the cellular process would be four fold larger than that of the cell body ;!ashley 188%< This difference in volume between the cell body and the process is even greater if the situation with cuboidal or flattened odontoblasts is considered, as seen in the root towards the ape* )t is generally agreed that the process of most odontoblasts is between & 1 and 1 &mm ;:yers 188%< The 3uestion of how far the odontoblast process penetrates dentin is of vital importance when considering dentin sensitivity )f odontoblasts were to participate directly in the sensitivity of dentin to surface stimuli, then the stimuli must interact directly with the process, which is unlikely to be the case 1ormally dentin is covered coronally with and on the root surface by cementum Bhen these surface coverings are lost, dentin is sub.ected to a variety of stimuli, including mechanical, chemical, thermal and smaller mechanical stimuli to which intact teeth are responsive Bhen e*posed, it is proposed that the fluid filled tubules allow minute fluid shifts across the dentin when e*posed to thermal, tactile, evaporative or osmotic stimuli The effect of this is that mechanoreceptors in the pulp are stimulated ;!ashley 188%< These fluid shifts can directly irritate odontoblasts, pulpal nerves and sub odontoblastic blood vessels by applying large sheer forces on their surface as the fluid streams through narrow spaces The effect of fluid shift on the release of neuro peptides has been assessed ;Limberly and :yers 1877, :yers et al 188&, :yers 188%<, and results in the release of calcitonin gene related peptide ;C0#!< or substance p ;S!< from the pulpal nerves to generate a local neurogenic inflammatory condition Dentin C#aracteristics C#an$e 2it# Dept#

2,

:oth primary and secondary dentin contains tubules The circumference of the dentin at the most peripheral part of the crown or root is much greater than that of the final circumference of the pulp chamber or root canal space this results in the odontoblasts being much more crowded as they approach their final position, thus leading to the appearance of a columnar layer of odontoblasts, especially over the pulp horns The convergence of odontoblasts towards the pulp creates a uni3ue structural organi9ation, with functional conse3uences The convergence has been estimated to be 2G1 The number of tubules per unit area and the radius of the tubules increases in the direction from the dentino/enamel .unction to the pulp, thus the area occupied by tubule lumina also increases !ashley ;1872< calculated the area occupied by tubule lumina at the dentino/ enamel .unction to be appro*imately 1= of the total surface area of the dentino/ enamel .unction and ((= of the pulp +s this area is occupied by dentinal fluid, which is 84= water ;!ashley 188%<, the surface area figures are also appro*imately e3ual to the tubule water content of these regions Therefore, the water content or wetness of dentin increases (& fold from superficial to deep dentin This factor has clinical implicationsE in terms of dentin bonding of restorative materials to deep dentin the water competes with resin monomers for surface collagen fibrils ;!ashley and Carvalho 1885< Flui! Flo. )n clinical conditions there is an outward fluid flow across e*posed dentin in response to the low but positive pulpal tissue pressure The composition of this fluid is uncertain, but must have an ion product of calcium and phosphate, which is above or near the solubility product constants for a number of forms of calcium phosphate ;!ashley 188%< This would in turn lead to the formation of mineral deposits in dentinal tubules which have many forms ;M.or 1874<, as the dentinal fluid moves outwards, larger amounts of mineral ions are presented to the walls of tubules than would occur in
22

sealed tubules )ndeed, Shellis ;1882< used this principle to reduce the depth of deminerali9ation in vitro under stimulated caries forming conditions, by using a supersaturated surrogate dentinal fluid, which was perfused through the pulp chamber Bhen e*amined microscopically, translucent bands resembling sclerotic dentin were sometimes observed Clinically, patients who complain of dentin sensitivity report that a cold stimulus elicits a greater response than evaporative, tactile or osmotic stimulation ;>rchardson and Collins 1875< >utward direct fluid movement ;in response to cold< is far more effective at activation pulpal mechanoreceptors than is the inward movement of fluid ;seen following a hot stimulus< Dentin ermea-ilit( The structure of dentin is tubular, as previously stated, and it is this characteristic that provides the channels for the permeation of solutes and channels for the permeation of solutes and solvents across dentin The density of tubules per mm s3uare varies from 14,&&& at the dentino/ enamel .unction to %4,&&& at the pulp boundary be predicted from tubule density and diameters, due to the presence of intra tubular material such as collagen fibrils and minerali9ed constrictions of the tubules ;!ashley 188%< Dentin permeability can be subdivided into two broad categories ;!ashley 188%<G Transdentinal movements of substances through the entire thickness of dentin via dentinal tubules ;such as fluid shifts in response to hydro dynamic stimuli< )ntradentinal movement of e*ogenous substances into the infiltration of hydrophilic adhesive resins into deminerali9ed dentin surfaces during resin bonding or deminerali9ation of inter tubular dentin by bacterially derived acids ;Linney et al 1884<, where the material enters the tubules but does not travel across the tubules

24

The presence of the smear plugs and J or intra tubular deposits ;i e sclerotic dentin< is thought to lower intratubular permeability to minimal values ;!ashley et al 1881< Dentin permeability ;Transdentinal or intratubular< is not uniform across the tooth Coronal dentin permeability is much higher than that of the root This can be attributed to the convergence of tubules towards the pulp chamber, the tubule density increases about four fold in coronal dentin, but only two fold in root dentin

Thus, within any location on the tooth peripheral dentin has a lower permeability than deeper dentin The permeability of intertubular dentin has never been 3uantified, but it must be very low and limited to patent lateral canals that branch off from tubules ;Chappell et al 1882, M.or and 1ordahl 188%< 1umerous methods have been used to assess dentin permeability ;!ashley 188&< The easiest method of measuring trans dentinal permeability is to 3uantify its hydraulic conductance This measures the ease with which fluid can filter across a unit surface area of dentin in a unit time under a unit pressure gradient ;!ashley 188&< )t has been reported, in unobstructed dentin, that the hydraulic conductance increases as dentin thickness decreases "owever, the presence of intratubular dentin and hence lowers its permeability ;!ashley 188%< The structure of dentin makes it act both as a barrier and a permeable structure, depending on its thickness, age and other variables ;!ashley and !ashley 1881< Dentin is very porous because of its tubular structure and the minimum porosity of normal peripheral coronal dentin is about 14&&& tubules per s3uare )f the dentin is uncovered, then the tubules provide a diffusion channel from the surface to the pulp

2%

The rate at which diffusional flu* of e*ogenous material crosses dentin to the pulp is highly dependent on dentin thickness and upon the hydraulic conductance of dentin ;!ashley 1874, 188&< T#e ulpo&Dentinal Comple1 Dentin and pulp are embroyologically, histologically and functionally united and there is much evidence to support the concept of viewing the dentin and pulp as a functionally coupled unit, which act as an integrated system +s soon as the tissues, which normally cover dentin, are lost, then normal compartmentali9ation between the tissues is lost ;!ashley 188%< and they become functionally continuous The pulp responds to the stimuli generated by the loss of dentinal covering, in the short term, by mounting an outward movement of fluid ;6ongsavan 1882, Mathews 188%< and macromolecules ;:yers 188%< The long/term response to the stimulus is the production of tertiary dentin, which is a biological response to reduce the permeability of the dentin of the dentin $pulp comple*

25

ACID ETCHIN" ON ENAMEL

The developed materials that adhere or bond to tooth structure would minimi9e removal of healthy tissue, thus allowing a more conservative preparation and providing for an impenetrable seal at the margin between the tissue and restoration Criteria for %on!in$ Three basic criteria necessary for bonding The surface with which the bonding is to occur should beG 1G Similar to the surface (G 'ree of contamination ,G Smooth and uniform

Steps In Aci! Etc# Tec#ni3ue

Enamel rop#(la1is The mechanical cleaning of the enamel is an important first step clinically in the bonding procedure Ma*imum bond strength was developed only when an oral prophyla*is was done before etching +n e*amination of etched enamel surfaces not receiving an oral prophyla*is shows pellicular remnants and microorganisms contaminating the enamel Clearly, acid alone cannot remove all contaminants This especially true of calculus and a careful inspection should be made for the presence of this accretion which should be removed by scaling
27

:ecause there is concern for interference of flavoring oils, glycerin and fluorides with the etching process, the use of watery slurry of flow pumice has been recommended There is no significant difference in the retention rate of sealants with or with out pre/etch pumice prophyla*is ;Donnan and :all 1877< "owever, no clinical or laboratory evidence has been presented to preclude the use of commercial pastes, !re operative / silver amalgam restoration cavity even those containing fluoride Studies in 187&Cs have +fter showed no preparation difference in the clinical performance of a sealant whether fluoridated or non/fluoridated toothpaste was used for the prophyla*is 'urther research is indicated ellicle Remo/al +n oral prophyla*is should remove all gross deposits and accretions from enamel, but it may not remove all integuments such as subsurface pellicle )n addition, some protein may become smeared over the surface during the prophyla*is +cid Etching #insing with water Some of this pertinacious constituent may go into the solution in the acid while the remainder may be floated away mechanically as the phase of enamel is solubili9ed Application of Etc#ant 4FI"5 678 )n the ne*t step, with the teeth dried and properly isolated from saliva, the acid is applied by one of several means including a cotton pellet, brush or minisponge The :lot e*cess water using mini sponge +pplication of bonding agent ob.ect is toor gently agitate the acid for a minute for ma*imal effect This can be cotton achieved using a gentle swabbing motion Clinical reports have suggested e*tending the etching time upto ( minutes in relatively high fluoride areas and highly calcified mature enamel as for an adult

28

!lacement of composite restoration

'ig 2&

'inished composite restoration

)t is important not to rub the enamel during acid application, since burnishing the friable rods and their crystallites will reduce the surface area available for
4&

bonding This has been shown to reduce bond strength Scrubbing or rubbing may push the decalcified material back into the pores that are being formed 1o apparent difference e*ists in the degree of irregularity after etching acid solution compared with an acid gel 0els provide better control for restricting the This gel is syringe etch area but may re3uire more through rinsing afterward The most popular enamel J dentin etchant in general dentistry is phosphoric acid blue gel dispensed, as ade3uate colour contrast, smooth consistency and almost ideal viscosity for application and rinsing off cleanly, and provides and even, nicely demarcated white frosted appearance This etchant is recommended whenever e*tra good etching of enamel is desired, such as deciduous teeth Studies and clinical e*perience indicate the 14 seconds is probably ade3uate for etching most young permanent teeth "owever, individual variation e*ists in enamel solubility between patients, between teeth, and with in the same tooth, and ,& to %& seconds may recommended for molars and adult teeth -onger periods provide no more, but actually less, retention because of loss of surface structure Caution should be e*ercised when etching over ac3uired and developmental deminerali9ation )t is best to avoid it )f this is impossible a short etching time the applicant of the sealant, and the use of direct bonding with e*tra attention to not having areas of adhesive deficiency are important The presence of avoids, together the poor oral hygiene, can lead to indelible staining of underlying developmental white spots

2as#in$ There is a significant increase in bond strength values when enamel is washed for %& secs compared to 14 secs These observations were made using phosphoric acid in concentration of ,&= and lower The chemical composition of the rinsing solution did not affect the bond strength 1= potassium Chloride solution was found to improve bond strength The presence of contaminants in the post etch rinsing solutions could adversely affect the composite bond strength 0iven the si9e of dentinal tubules any contaminant that is small enough to penetrate or obstruct the flow
41

of monomers into the dentinal tubules may influence the process of polymeri9ation and ultimately affect the development of hybrid layer and potential bond strength Significant reduction in the bond strength was demonstrated when saline was used as rinsing solution, due to the presence of ions, which interfered with the formation of hybrid layer ;Eric C Sung et al (&&(< )n clinical procedure involving the etching of dentin with phosphoric acid, it re3uires complete removal of etchant and reaction products that are formed on the etched dentin surface, as in complete removal of reaction products will intervene with bond strength ;:ates et al 187(< +t the end of etching period the etchant is rinsed off the teeth with abatement water spray + high/speed evacuator is strongly recommended for increased efficiency in collecting the etchant / water rinse and to reduce moisture contamination on teeth and Dri/+ngles Salivary contamination of the etch must not be allowed ;)f it occur, rinse with the water spray or re/etch for few secondsE the patient must not rinse<

Dr(in$ 1e*t, the teeth are thoroughly dried with a moisture/and/oil/free air source to obtain the well/known dull, frosty appearance frosty white should be re/etched a sufficiently etched tooth Teeth that do not appear dull and Cervical enamel, because of its different

morphology, usually looks somewhat different from the centre and incisal portions of )t should not be re/etched in attempts to produce a uniform appearance over the entire enamel surface

Effects Of Etc#in$ On Enamel

+ routine etching removes from , to 1&m of surface enamel +nother (4m reveals subtle histologic alterations, creating the necessary mechanical interlocks Deeper locali9ed dissolution will generally cause penetration to a depth of 1&& m or
4(

more +lthough laboratory studies indicate that enamel alterations are largely ;though not completely< reversible, it can be stated that the overall effect of applying etchant to healthy enamel is not detrimental This is augmented by the fact that normally ;e*cept as it tapers toward the cervical enamel is from 1&&& to (&&&m thick

margin<, abrasive wear of facial enamel is normal and proceeds at the rate of upto (m per year, and facial surfaces are self/cleaning and not prone to caries >n the other hand, caution should be e*ercised when etching damaged teeth with e*posed dentin, deep enamel cracks or e*ternal or internal deminerali9ation attern of Etc#in$ Silverstone et al ;1854< studied the morphological changes produced on the acid etched enamel surface scanning electron microscope E*posure of human enamel to conditioning solutions produces three basic etching patterns ;')0 2(a< 'ig 21 Etching pattern of enamel after acid etching

Type )

Type )) 'ig 2(a Different types of etching pattern

Type )))

4,

'ig 2(b +cid etched enamel rod core dissolved to greater e*tent than rod sheath

T(pe ) !rism core material is preferentially removed, leaving the prism peripheries relatively intact, resulting in a honeycomb appearance ;')0 2(b< The average diameter of the hollowed prism cores measures about ,Mm This pattern is most common of the three types observed T(pe + The peripheral regions of the prism are dissolved preferentially, leaving the prism cores relatively intact, resulting in a cobblestone appearance T(pe * Etching pattern contains areas, which resembles both type 1 and type ( along with some distinct areas where the pattern of etching appears to be unrelated to the enamel prism morphology Studies with polari9ed light microscope showed that sound enamel etched with phosphoric acid to be affected at , distinct levels and may be described in terms of three specific zones ;Silverstone 1852< A superficial etched zone, which is a narrow 9one of enamel of about 1& microns in depth that is removed by etching A Qualitative porous zone of about (& microns in depth )t is rendered porous by the acid attack and may be identified 3ualitatively using polari9ed light A Quantitative
42

porous zone of about (& microns depth that 3ualitatively indistinguishable form ad.acent enamel En#ancement of Enamel orosit( Enamel is a porous tissue that contains appro*imately & 1= to & (= by volume of space Many of the pores communicate to allow for transport of tissue fluid and ions in solution !oole and his coworkers ;18%1< showed that enamel behave like a molecular sieve, allowing passage of only the smallest molecules comparable in si9e to that of water +cid etching enhances not only the si9e of the pores to permit access of relatively large resin molecules, but does so far distances appro*imately (& to ,& micrometer in from the tissue surface Decreased concentration of phosphoric acid enhances porosity to greater depths in the enamel This observation holds significance for the depth to which resin may penetrate into the tissue Antimicro-ial ropert( of Etc#ants -settembrine et al ;1885< at the university college of dentistry 1ew Iork concluded that all phosphoric acid etchant materials tested demonstrated antimicrobial activity against several bacteria commonly found in the oral cavity They also reiterated that addition of antimicrobial agents to etchant or cavity preparation may not be necessary given the antimicrobial activity of the etchant, if the current bonding systems can provide and sustain sealed tooth restorative interface

Role Of Flouri!es In Etc#in$ Of Enamel

Enamel is soluble when e*posed to an acid medium, but the dissolution is not uniform Solubility of enamel increases from, the enamel surface to the dentino/ enamel .unction Bhen fluorides are present during enamel formation or are topically applied to the enamel surface, the solubility of the surface enamel is decreased 'louride concentration decrease towards the dentino/enamel .unction
44

'louride

additions can affect the chemical and physical properties of the apatite mineral and influence the hardness, chemical reactivity, and stability of enamel while preserving the apatite structures Trace amount of fluorides stabili9e enamel by lowering acid solubility, decreasing the rate of deminerali9ation and enhancing the rate of reminerali9ation Evidence also shows that topical fluorides alter the oral bacterial flora, there by increasing resistance to dental caries )t has been accepted to etch apparently normal enamel for 14 secs and enamel that shows signs of fluoridation for double that time or more The use of prophyla*is pastes containing fluorides and topical fluoride treatments prior to etching is slowly diminishing There is virtually no evidence that the fluoride incorporated in enamel prior to etching will significantly interfere with etching or will significantly affect bond strengths )t is well known that even the fluoride/ac3uired from acidulated topical fluoride solutions is poorly retained and easily removed under oral conditions in a short time There is no contraindication to the use prior to etching because the fluoride from these agents including acidulated or nonacidulated sodium fluoride and stannous fluoride, will most likely find its way into the deep recesses of the pits and fissures and benefit in sealing them This solid fluoride may conceivably be retained in the pits and fissures even after etching >nce sealed in the fissure by a sealant, the fluoride may gradually react with enamel ;and perhaps with dentin, which in accessible at the base of some fissures< to produce a resistant tooth structure that can afford protection against caries even when sealant application is no longer provided 'luorides should be avoided as part of the etching solution or immediately prior to regular bonding Studies have shown that fluorides react with etched surface to produce reaction products that may interfere with bonding These reaction products appear to interfere with optimal adhesive penetration resulting in weaker bond andJor bonds that will not survive as long under conditions of oral moisture )t should be noted that washing away the acid conditioning solution

4%

with water containing 1or ( parts per million of fluoride is not e*pected to interface with achieving high bonding strengths Upta9e of Fluori!es in Etc#e! Enamel Most important use of fluoride is after bonding procedures of all types During etching more enamel surface usually is intentionally or unintentionally etched than is subse3uently covered by adhesive, such as inter pro*imal areas etched by acid spillover Etched enamel is highly reactive and readily combines with and better retains many times more fluoride than a natural unetched enamel surface The large amount of fluoride thus ac3uired by etched but uncovered enamel from a topical fluoride application, may confer on the etched enamel surface a greater resistance to cavities, normally have this capacity )nfact, it has been suggested that a mild acid etch ;independent of bonding procedures< be employed prior to application of acidulated sodium fluoride in order to enhance the ac3uisitions and retention of fluoride from this source #etief et al ;187%< has stated that fluoride is not evenly distributed through out enamel, the fluoride concentration follows a negative e*ponential distribution being highest in the surface enamel environment The loss of fluoride rich surface enamel during the etching procedure may make the enamel more caries susceptible in the oral

Factors Affectin$ Etc#in$ On Enamel

TIME Increase! Time Application "igh fluoride content and primary teeth re3uire longer etching time The

increased etching time is needed to enhance the etching pattern on enamel that is more
45

a prismatic than that of permanent enamel Currently 14 sec, a sufficient time to produce a bond e3uivalent to that produce by a %& sec etching time is used routinely S#orter Etc#in$ Time C F 0uba et al ;1882< highlighted that etching times and etchant consistency were not critical to enamel bond strengths conserves enamel and saves time They also found that on microscopic e*amination of a 1& secs etch versus a %& sec etch showed that etching the enamel for 1& sec produced a very superficial etch compared to a very deep etch with a %& sec etch "owever this did not have significant impact on the tensile strength Though some researchers suggested that the etching effect is reduced when the etching viscosity of the acid is high, this study showed no significant difference as related to their viscosities ACID CONCENTRATION +n interesting and important phenomenon is the e*istence of an inverse relationship between the etching effect of phosphoric acid and itCs concentration The phenomenon was first observed and reported in 18%4 and subse3uently confirmed by others The same etch time lower concentrations of acid tend to be more destructive of the enamel than higher concentrations ;')0 2,a to f< )t yields acceptable bond strength )t

47

'ig 2,a 1&= ",!>2

'ig 2,b ,(= ",!>2

'ig 2,c ,4= ",!>2

'ig 2,d ,4= ",!>2 for ( minutes

'ig 2,e ,%= ",!>2 for ,& secs

'ig 2,f ,5= ",!>2

Etching pattern with various concentration of phosphoric acid ;SEM<

Concentrations of phosphoric acid over %4= tend to show minimal changes The concentrations of acid, producing consistent, more or less evenly distributed relatively deep etch pattern, appear to be in the range of ,& to 4&= :ond strengths are greater with ,& to 4&= acid concentration, the difference between their values and those obtained on surfaces etched with 1& to 5&= acid were not as great The higher concentration of acid may not produce a sufficient in depth etch to provide ade3uate resin penetration ;tag formation< and J or sufficient bonding area to resist repeated long/term masticatory and other dislodging stresses encountered in the oral environment )n an in vitro study carried out on bovine substrate by M F Shingi et al ;(&&&< it was concluded that milder concentrations of phosphoric acid or less aggressive
48

acids could be used to pretreated enamel for orthodontics adhesive systems and sealants if the diffusion potential of applied monomers is high enough +ccording to ?nos ;188%< depths of deminerali9ation increased by both acid concentration and conditioning times following a logarithmic relationship Chow and :rown ;185,< demonstrated that the application of phosphoric acid solutions greater than (5= !hosphoric acid resulted in the formation of monocalcium phosphate monohydrate while dicalcium phosphate dehydrate was formed with phosphoric acid concentrations less than (5= The former product is readily soluble and would be completely washed away in the clinical situations

0ARIATIONS IN ACID ETCHIN" METHODOLO"IES

Currently phosphoric acid is the acid of choice, but it is possible that other acidic etching agents such as pyruvic acid may be used in the future + controversial issue, however, is the optimal concentration of phosphoric acid phosphoric acid The most widely used concentrations of phosphoric acid used in clinical practice e*ceed ,&= This is partly based on the findings the phase diagram of the phosphoric acid calcium hydro*ide water ternary system They demonstrated that the application of phosphoric acid solutions greater than (5= phosphoric acid resulted in the formation of monocalcium phosphate monohydrate phosphoric acid Bhile dicalcium phosphate dihydrate was formed with phosphoric acid concentrations less than (5= The former product is readily soluble and would be completely The washed away in the clinical situation, while the latter product is less soluble interfere with the bonding of composite resins to etched enamel surfaces

reaction products, if not completely removed after the etching procedure, may

%&

The effect of phosphoric acid concentration on the tensile bond strength of a conventional composite resin to enamel surfaces etched with 1&, (&, ,&, 2&, 4&, %&, and 5&= phosphoric acid was determined The tensile bond strength to enamel surfaces etched with 5&= phosphoric acid was significantly lower than the bond strengths recorded to enamel surfaces etched with other phosphoric acid concentrations The application of a phosphoric acid etching solution to freshly cut dentin may elicit a pulpal response To prevent the flow of phosphoric acid applied to the enamel walls of preparations to the freshly e*posed dentin at the floors of the preparations phosphoric acid gels were recently introduced The ob.ective was to confine the acid/ etching agent to the intended site of application )t is recommended that the etching agent should be applied to the enamel surface using a dabbing action as opposed to rubbing +nother issue that has not been resolved is the optimal duration of etching with phosphoric acid )t is surprising that some authors recommend that the etchant should remain on the tooth surface for at least %&seconds to develop an appropriate etched pattern The etch duration is of bonding site particular importance in acid etching enamel prior to the direct bonding of orthodontic attachments, as it is practically impossible to confine the 'luoride is not evenly distributed in enamel but allows a negative e*ponential distribution with fluoride concentration being in the surface enamel The loss of fluoride rich enamel surface during prolonged etching may make the ad.acent enamel more susceptible to enamel decalcification during orthodontic treatment The reaction products that are formed on the enamel surface after phosphoric acid etching should be removed completely, as incomplete removal may interfere with bond strength Etched surface should be washed for at least 14 secs to remove the reaction products The tooth to be restored should be isolated with a rubber dam to prevent saliva contamination prior to acid etching and the placement of composite resin )t is generally recommended that saliva contaminated etched enamel should be washed and retched >C:rien and others showed, however that it was not necessary to re/etch
%1

an enamel surface contaminated briefly with saliva, as a thorough washing of such a surface did not have a detrimental effect on bond strength :uonocore M ;1844< introduced a simple conservative techni3ue for bonding restorative resins to enamel "e placed a drop of self/curing acrylic resin on the labial enamel surface of upper central incisor of ten sub.ects >ne surface was treated prior to resin placement with 74= phosphoric acid for ,& seconds "e noted that the acid conditioning of the enamel resulted in on uncontioned control surfaces lasted less than 1( hours +fter three decades of laboratory and clinical research, :uonocoreCs method is widely adopted and has added a new and e*citing technical dimension to the practice of dentistry 0winnett, Matsui and :uonocore ;18%8< suggested that formation of resin tags was the primary attachment mechanism of resin to phosphoric acid +cid etching removes about 1& microns of the enamel surface and creates a porous layer ranging from 4/4& microns deep Bhen a low viscosity resin is applied, it flows into the micro porosities and channels to this layer and polymeri9es to form a micro mechanical bond with the enamel 'usayama et al ;1858< introduced an etching techni3ue for both the enamel and the dentin cavity wall using ,5= phosphoric acid followed by a dentin/bonding agent containing methacrylo*yethyl hydrogen phenyl phosphate ;phenyl/!< This improved bond strength greater e*tent and dentinal etching has become fairly common practice in Fapan "owever, the concept of total etching only recently has gained acceptance in the ?nited States

%(

ACID CONDITIONIN" OF DENTIN

+ny discussion of the effects of acid conditioning of dentin must begin with the acid etching of enamel This was first proposed by :uonocore ;1844< as an attempt to clean enamel, increase the microscopic surface area for bonding, and infiltrate unfilled resins into enamel porosities Many investigators were alarmed at what was then regarded as an unconventional and even reckless approach to the problem :uonocore, Bilernan and :rudevold ;184%< not only introduced the acid etching of enamel to dentistry, they also were among the first to attempt to bond resins to acid/etched ;5= "C-, one minute< dentin Their success with acid etching of enamel led them to try to acid etch dentin ?nlike enamel, when dentin is etched, its surface becomes mineral /poor protein richE and it tends to become wetter ;:rannstrom and 1ordenvall 1855< ?nfortunately, :uonocore and his colleaguesN success with dentin was never reali9ed, because the relatively crude resin materials that were available at that time would not wet dentin very well :uonocore, however, was very much aware or the re3uirements for good bonding 'or clinical success, the conditioned dentin must be sealed to prevent sensitivity and to prevent the pathology ;:rannstrom, 1871< associated with the increased permeability of the dentinal tubules Conditioning of dentin will be defined as any alteration of dentin done after the creation of dentin cutting debris, termed the smear layer The ob.ective of dentin conditioning is to create a surface capable of micro/ mechanical and possible chemical bonding to a dentin/bonding agent "oals of aci! con!itionin$ of !entin #emove the intrinsic weakness of the smear layer to permit bonding to underlying dentin
%,

Deminerali9e the superficial dentin matri* to permit resin infiltration into surface ?ncover both intertubular and peritubular dentin Clean the dentin surface free of any biofilms )t is important to define the purpose of the acid etching of dentin so that once

identified, these goals can be tested in a systematic scientific manner +s the smear layer is intrinsically weak, the first goal is to loosen it or remove it so that subse3uently placed adhesive resins can interact with solid dentin adhesive resins can interact with solid dentin matri* Most smear layers are 1/( Mm thickE they are composed of the cutting debris of the materiali9ed tissue on which they lie ;#use and Smith 1881< The reason for acid etching is to deminerali9e the solid dentin matri* ;both intertubular and peritubular dentin< to increase the porosity of the dentin Bhile this is analogous to why enamel is etched, the porosities that are produced are of the order of & &4 $ 1/, Mm in peritubular dentin rather than the 4/5 Mm diameter of enamel prisms 'urther, acid/etched enamel can be thoroughly dried, while that foal is much more difficult in vital, normal dentin Enamel contains little protein that is at risk of being denatured by acid treatment Dissolving away hydro*yapatite mineral crystallites from the collagen component of dentin matri* creates dentin porosities The crystals tend to stabili9e collagen and prevent its denaturation There is a risk that the acid used to deminerali9e the dentin may denature or weaken the collagen +s denatured proteins generally change their dimensions, the pores may become smaller if the collagen is denatured This may interfere with subse3uent resin infiltration and prevent the formation of a hybrid layer ;1akabayashi, 1akamura and Iasuda 1881< +nother danger in the etching step is that the deminerali9ed 9one may e*tend, for instance, 4 Mm into the dentin, while the resin infiltration may only e*tend 2 Mm, leaving a 1 Mm deminerali9ed 9one at the base of the hybrid layer that is unprotected by mineral or resin and that may be structurally weak )f the pulpodentin comple* can re/minerali9e this unprotected
%2

basal 1 Mm of deminerali9ed dentin ;Tatsumi, 1878E Tatsumi and others 188(<, then the layer may become as strong as normal dentin, rather than be a 9one of debonding that has been seen in vitro ;1akabayashi and others 1881< +nother purpose of acid etching dentin is to clean the dentin surface >ften dentin is inadvertently contaminated with blood during the cavity preparation +cid etchant, by dissolving most of the smear layer, tend to float these biofilms on the dentin when it is rinsed The low p" of the etchant may also denature the plasma proteins and hemoglobin The purpose of acid etching may vary depending upon the material )f the intention is simply to remove the smear layer but leave the smear plugs in place, as when one uses glass/ionomer cements, then short etching times with dilute acids would seem to be indicated ;:owen 1857E !ashley and >thers 1871E "amlin and >thers 188&a< "owever, if one wants to create a resin hybrid layer ;1akabayashi and >thers 1881< in the dentin rather than on the dentin, then one must deminerali9ed more deeply and in the process, removes smear plugs This can still be accomplished using dilute acids, but the etching time may have to be e*tended

Effects Of Con!itionin$ Of Dentin

The principal effects of conditioning of dentin may be classified as a< b< !hysical changes Chemical changes

#(sical c#an$es )ncreases or decreases in the thickness and morphology of smear layer changes in the shape of dentinal tubules C#emical c#an$es a< Modification of the fraction of organic matter b< Decalcification of the inorganic portion
%4

Conditioning of dentin may be done by several means 1< Chemical a< +cids b< Calcium chelators (< Thermal a< -asers ,< Mechanical a< +brasion Bhen dentin is cut for cavity preparation, the wrenched cutting debris of the dentin forms a thin smear layer on the surface )t is also driven into the dentinal tubule apertures displacing the odontoblast process and forming a smear plug at a depth of less than 1&/micron meter Etching dissolves the smear layer and part of the peritubular dentin, leaving tapered cylindrical holes of that depth )n an e*periment on monkey, dentin wall deminerali9ed with a phosphoric acid .elly etchant for %& sec was completely re/minerali9ed after 2 months This results indicates that etching did not result in deleterious effect upon either the collagen fibers or the odontoblast processes, because the presence of collagen fibers maintaining their proper cross bonded structure as a base for apatite crystals to attach to and of the vital odontoblast processes to supply the calcium phosphate from the pulp is essential for reminerali9ation of dentin + F 0winnett and M D Fendresen ;1857< have concluded from their e*periments and observations that the surface of acid conditioned eroded dentin is significantly different from that of acid conditioned normal dentin They further observed the depth of penetration of resin is also less in acid treated eroded dentin where many tubules remain partially occluded by intratubular insoluble deposits #use and Smith ;1881< found when common conditioning agents were used, it has been found by O/ray photo electron microscopy that the outermost surface contains only 1&= or less of the calcium and phosphorus initially present They concluded that the treatment of dentin with acidic conditioners leaves the surface so depleted of calcium and enriched by organic residues that subse3uently placed
%%

bonding systems should be based upon agents able to interact with organic components of dentin :onding agents that rely on chelation to calcium are unlikely to be successful when applied to acid etched dentin unless they penetrate into the deminerali9ed matri* to reach normal, minerali9ed dentin +cid etching of dentin is not harmless but represents one more source of acute irritation to the pulpodentin comple* in addition to the vibratory, thermal, mechanical and evaporative stimuli that accompany cavity a preparation "owever, it is not as irritating as has been previously thought 1akabayashi ;187(< introduced the concept of hybridi9ation The techni3ue consists of applying an acid, ranging in concentration from 1&= to ,&= to the surface of dentin Bithin 14 minutes the acid selectively dissolves away the inorganic component of the dentin to a depth of 4 to 1& microns )t then flows in the dentinal tubule for up to 1&& microns at which point it diffuses laterally into the peri/tubular dentin for up to 1& microns +s in the previous case the calcium component is selectively eliminated Then these spaces are replaced by an insoluble resin component that completely encapsulates all e*posed collagenous fiber "e also reported that dentin conditioning by citric acid containing ferric chloride followed by a dentin bonding agent containing 2 MET+ ;methacrylo*yethyl trimellitate anhydride< was effective method of dentinal bonding Concerning the bonding mechanism, he proposed that diffusion and impregnation of monomers into the subsurface of pretreated dentinal substrate and their polymeri9ation, creating a hybrid layer of resin reinforced dentin This newly formed hybrid layer may be thought of as an admi*ture of polymer and dentinal components, creating a resin dentin composite This techni3ue not only enhances the shear bond strength of the resin to the dentin but also increase the potential against micro leakage and postoperative sensitivity 1akabayashi ;1874< suggested
%5

that

the

acidic

treatment

partially

deminerali9ed a 9one of the dentin near the surface, facilitating an infiltration process

of compatible monomers The polymeri9ed resin forms a reinforced 9one of dentin on which a resin based restorative material can be bonded The bond strength is not dependent upon interlocking at the dentinal tubules Lurosaki et al ;1875< found that etching of dentin of the clinical cavity floor allows the chemically adhesive composite resin to produce resin tags of tapered, cylindrical or tubular form as well as impregnated dentinal layers These changes will considerably improve the bond strength as well as the tubule aperture seal Surface Interactions Of Dentin Con!itioners Smear la(er remo/al >ne purpose of a dentin conditioner is removal of the smear layer to provide a surface that is more suitable for adhesionE however this does not necessarily apply to all systems 'or e*ample, the +ll/:ond system can be used with the S+/"EM+ conditioner, which is weakly acidic and probably modifies the smear layer without removing it, e*cept where the smear layer is 3uite thin Dentin permea-ilit( c#an$es #emoval of the smear plugs results in increased permeability of the dentin, and the rate of removal by conditioner can be e*amined by measurements of permeability increase for different application times This is controlled by the strength of the acid, itCs concentration, and whether there are modifying components in the conditioning solution ;')0 22< :ecause acid etching increases dentin permeability and dentin wetness, successful bonding at adhesive resins to acid etched dentin re3uires the use of hydrophilic resins that bond e3ually well to both peritubular and intratubular dentin 'uture trends seem to be toward lowering both the concentration of acids and the time of etching dentin Conditioner +pplication Time To +chieve Ma*imum !ermeability
%7

C>1D)T)>1E# ( 4=1itric +cid %=Citric +cid ,5=!hosphoric acid ( 4=Maleic +cid 44="EM+

Time ;sec< P1&/ Q14 P14 P%& Q1(

Deminerali'ation of !entin surface -( con!itionin$ a$ents Conditioning agents not only remove the smear layer, but also cause deminerali9ation of the underlying dentin Complete loss of peritubular dentin occurred 14 microns deep when ,5= phosphoric acid was applied for %& seconds Deminerali9ation depths of 1&/14 microns may be greater than monomers can effectively penetrate Deminerali9ation of dentin to a depth greater than monomers can infiltrate and reinforce the collagen network can lead to decreased adhesion ;1akabayashi 1878E Liyomura 1875< Bhen the 0luma system was used with various acid conditioners, bond strength decreased with decreasing !" of the acid used ;+smussen and :owen, 1875< ;')0 24< Similarly, bond strength has been found to decrease as dentin surface hardness decreases when acid concentrations and self/etching primers of various strengths are used ;Chiba, )toh and Bakumoto 1878E )ngaki and >thers< Surface hardness gives an indication of surface deminerali9ation, and a %& second treatment with phosphoric acid of ,&/24= concentration can reduce the surface hardness to 14/,&= of its initial value and cause deminerali9ation of greater than 1& micron deep )n another study, complete loss of peritubular dentin occurred with 14 micron deep when ,5= phosphoric acid was applied for %& seconds ;Erickson and others 1881< Deminerali9ation depths of 1&/14 micron may be greater than monomers can effectively penetrate Cadiaco Mc et al has revealed that both 1&= maleic acid and

%8

,%= phosphoric acid completely the smear layer and deminerali9ed the dentin, leaving a layer of collagenous network Effect on colla$en Conditioning agents may also affect collagen of the dentin surface 1akabayashi ;1874, 1878< has shown that the conditioning dentin with phosphoric acid and citric acid resulted in low bond strengths when used with the 2MET+JMM+J/T:: adhesive systems "owever, addition of ferric chloride to the conditioner improved the bond strength drastically, and this was attributed to stabili9ation of the collagen by ferric ions during etching )t has been shown that phosphoric acid denatures collagen fibers are still surrounded by hydro*y apatite crystals because of their buffering capacity ;')0 2%a,b< Alteration of surface .etta-ilit( :ecause wettability of the surface is the first re3uirement of adhesion, it is of interest to e*amine the effect that dentin conditioners have an effect on surface wet ability Dentin with a smear layer has been found to have a critical surface tension of wetting ;:enediktson1881< 'ollowing reduced to (5 (5dynesJcm conditioning surface with EDT+ solution of 0luma was reduced to (8 27 dynesJcm and similarly, the conditioner of Tenure

Erickson in 1878 studied the surface region of specimens where all bond systems has been applied with the techni3ue using 1&= !hosphoric acid as a conditioner There were numerous resin pro.ections from the tubular tags that represent penetration into lateral canals and indicate the good wetting Smear la(er

5&

The smear layer, an incidental conse3uence of cavity preparation with rotary instruments, has been the sub.ect of considerable investigation The particles that remain on the surface of dentin after tooth preparation vary in si9e from & &4 to 1&Mm +lthough they tend to be irregular, the larger particles have plate like con.urations to stack into a layer that is seldom more than 1Mm thick The composition of these particles is similar to the dentin form, which they are formed )ntentional removal of the smear layer during restorative procedures is controversial ;')0 25< >ne school of thought suggests that because the smear layer occludes the dentinal tubules, it precludes bacterial invasion >thers advocate removal of the smear layer to enhance the bonding of adhesive restorative materials and encourage the ingress of tags into the enlarged orifices of the dentinal tubules + further argument in favour of removal is that the smear layer, although composed primarily of inorganic material, may have a significant organic component including viable bacteria and their byproducts that might provide a reservoir of irritants Thus complete removal of the smear layer would be consistent with the elimination of irritants Bhen normal dentin is cut with a bur, grinding debris is forced into open tubules to form smear plugs of variable length 'urther their grinding debris is burnished over the smear plugs to form a smear layer The combination of smear layer and smear plugs forms a physiologic unit that is responsible for reducing the permeability of prepared dentin The length of the smear plugs may depend on the diameter of the tubules Dentinal tubules are inverted cones with the bases at the pulpal surface of dentin Thus, one would e*pect deep dentin to have longer smear plugs than superficial dentin with smaller diameter tubules ;6an Meerbeek and others, 188(< )f the smear plugs are so long that the hydrogen ions in the acidic primers cannot reach them in the typical ,&/ %&/second application time, then these agents could remove the smear layer but does not increase dentin permeability )f these primers remove both the smear layer and smear plugs then dentin permeability will increase to near ma*imum values +dditionally, resin tags of varying lengths with obviously penetrate
51

further into tubules that are devoid of smear plugs than in tubules containing residual plugs " Loibuchi et al ;(&&1< concluded that self etching prime can provide an effective alternative to conventional phosphoric acid etchant in conditioning the enamel surface to secure a durable bonding and marginal seal of composite resin restoration, tested on bovine enamel and demonstrated 3uiet clearly that hybridi9ed dentin indeed form beneath resin impregnated smears which bonds well for bond longevity and prevention of no*ious stimuli from reaching the pulp Self/etching bonding systems that function with intact smear layers greatly simplify clinical adhesion procedures They however recommended delaying final .udgment until more clinical evidence is obtained

The mineral component of the smear layer can be dissolved in a few seconds of etching, depending upon the pLa of the acid, its p", chemical concentration and viscosity The collagen phase of the smear layer is acid, insoluble and presumably remains on the etched surface Effect of smear la(er on -on! stren$t# The retention of smear layer not only lowers dentin permeability ;!ashley, Michelich and Lehl, 1871< but may prevent the decrease in bond strength seen with some bonding systems as deeper dentin is prepared ;!rati, !ashley and Montanari, 1881E Tao, Tagami and !ashely, 1881< )t also greatly lowers the effects of pulpal pressure on bond strength ;Tao and !ashely, 1878< Thus, there are many reasons to retain smear layer as bonding substrate Some investigators recommend that the smear layer be removed with various acids to optimi9e the bonding of restorative materials to dentin, while others feel it can be left but modified, since its presence reduces the permeability of dentin ;Stanley, 1878E :rannstrom, 1871E Schulein, 1877< ;')0 25< Effect of c#emical con!itioners on smear la(er

5(

)nokoshi and others ;1878< have investigated the effects of a wide range of dentin conditioners and bonding agents This study has demonstrated differences in the depth of dentin decalcification as well as the thickness of the resulting hybrid ;dentin and resin< layers The hybrid layer results when resins are applied to conditioned dentin +ll the conditioners investigated are capable of removing the smear layer, but not all will remove the plugs from the tubules The chemistry of the applied conditioner was subse3uently shown ;Sui9aki, 1881< to affect the thickness of decalcified 9one the resulting hybrid layer This may be due to interaction with collagen in the outer

'ig 22 )ntertubular porosity

'ig 24 +cid conditioning stage

+
'ig 2% +

SEM of etched dentin showing e*posed collagen fibers, : + higher magnification showing collagen banding

5,

'ig 25 )mpregnation of smear layer

'ig 27 SEM of a smear plug blocking entrance of dentinal tubule

Moist /ersus !r( !entin surface 6ital dentin is inherently wet, therefore, completely drying of dentin is difficult to achieve clinically Bater has been considered an obstacle for attaining an effective adhesion of resins to dentin The @wet $bondingA techni3ue prevents the spatial alterations ;i e , collagen collapse< that occur upon drying deminerali9ed dentin ;')0 28< Such alterations may prevent the monomers from penetrating the labyrinth of nano channels formed by dissolution of hydro*yapatite crystals between collagen fibers The wet bonding techni3ue has been shown repeatedly to enhance bond strengths because water preserves the porosity of collagen network available for monomer interdiffusion )f the dentin surface is dried with air, the collagen undergoes immediate collapse and prevents the resin monomers from penetrating Bhen etched dentin is dried using an air syringe, bond strength decrease substantially, especially for acetone and ethanol based dentin adhesive system Bhen water is removed, the elastic characteristics of collagen may be lost The collapse of the collagen fibers upon drying may therefore be a result of the change in the molecular arrangement Bhile in a wet state, wide gaps separate the collagen molecule from each other, in a dry state, the molecules are arranged more compactly ;')0 4&< This is because e*tra fibrillar spaces in hydrated Type 1 collagen are filled with water, while dried collagen has fewer e*tra fibrillar spaces open for the penetration of the monomers included in the adhesive systems During air drying
52

water that occupies the interfibrillar spaces previously filled with hydro*yapatite crystals is lost by evaporation, resulting in a decrease of the volume of the collagen network to appro*imately to one $third of itCs original volume Bhen air/dried deminerali9ed dentin is rewet with water, the collagen matri* may ree*pand and recover its

'ig 28 Moist dentin surface $ Dynamics

'ig 4& Collapse of etched dentin by air drying

54

'ig 41 Etching pattern of dentin, etched with maleic acid

primary dimensions to the levels of original hydrated state This spatial ree*pansion occurs because the spaces between fibers are refilled with water and because Type1 collagen itself is capable of undergoing e*pansion upon rehydration

Factors Affectin$ Dentin Con!itionin$

TIME Duration of application :rannstrom and his colleagues achieved good bonds of resin to dentin using a five/second application of ,5= phosphoric acid ;:rannstrom, Fohnson and 1ordenvall, 1858< !erhaps ,& seconds of 4= !hosphoric acid would have been e3ually effective The same agent may remove the smear layer in five seconds can cause considerable decalcification if left in place for ,& seconds and produce pulpal damages began to appear using less concentrated acids with higher molecular weights and shorter time intervals, such as tannic acid (4=, poly acrylic acid (4=, deducing & &8= ;power D other, 187(E 6an de 6oorde, 0erdts and Mue*hision 1877< buffered formic acid and ( butyric acid ;M.or and >thers 187(< which produced minimal pulpal responses Tagarni and >thers ;1888< Compared a series of acids for their ability to clear tubules of smear layers and smear plugs by measuring the increase in the hydraulic conductance of smear layer/covered dentin as a function of etching time !resumably, the same amount of deminerali9ation was occurring in intertubular dentin :losser and >thers ;1878< reported that etching normal dentin for (&/,& seconds with ( %= nitric acid was as effective at was as effective at removing the smear layer and opening up dentinal tubules as 4& or %& seconds of etching
5%

Etching times may also need to be ad.usted when attempting to etch sclerotic dentin such as e*cavated carious dentin or abraded cervical root surfaces Dluke and -indemuth ;188&/1881< have shown that this dentin is much less etchable and more resistant to acid attack than normal dentin !resumably, this is because much of it is made up of whitlockite, a relatively acid/resistant form of calcium phosphate Thus the etching conditions re3uired to create a hybrid -ayer in sclerotic de tin have not yet been demonstrated )n an in vitro study conducted at the university of )stanbul faculty of dentistry the following conclusions were obtained :enderli ;1888< The application of strong acids ;ferric chlorideJcitric acid or phosphoric acid to a dentin surface for 14 secs significantly gave higher bond strength values than %& secs applications +pplying weak acids ;maleic acid or 1a/EDT+< to dentin for 14 secs significantly decreased the bond strength values compared to %& secs applications The highest value of the weakest acid and the lowest value of the strongest acid ;phosphoric acid< for the same period ;%& secs< were not statistically significant The highest bond strength values were obtained with the application of maleic acid ;%& secs< or !hosphoric acid14secs or ferric chlorideJcitric acid 14 secs 1 :rannstrom and L F 1ordenvall ;1855< in their study showed that etching prepared cavities using ,5= phosphoric acid for ,& seconds and ( minutes had no demonstrable difference in appearance in enamel and dentin Though acid etching could open dentinal tubules, only incomplete tags were formed when enamel bond resin was forced into them This produced a restoration of insufficient marginal adaptation S#ortenin$ of application time of con!itionin$ a$ents )n 1855, :rannstrom and 1ordenvall noted demonstrable difference between dentinal surfaces etched for 14 seconds or two minutes and recommended shorter
55

etching times This appeared to be the beginning of a new phase in dentin conditioning Concentration I :enderli ;1888< studied the effect of various dentin acid treatment on tensile bond strength of composite to dentin "e concluded that the application of strong acids such as ferric chloride or phosphoric acid to dentin surface for 14 sec gave significantly higher bond strength values than for %& sec application "e also stated that when weak acids such as maleic acid was applied for 14 sec to dentin showed decreased bond strength values compare with %& sec application This is because weak acids remove the smear layer after an increase in the etching time >n the other hand the strong acids remove the smear layer in 14 sec , when applied for a long time ;%& sec <, they removed both smear layer and peritubular dentin This causes the protein contents to rise to dentin surface resulting in bonding strength Effect of a!!iti/es +dditives to the acid solution can affect the rate of removal of smear layer and plugs as shown in table +ddition of 44= "EM+ to ( 4=maleic acid more than doubles the time re3uired to reach ma*imum permeability even though the measured !" is the same

This might be e*plained by absorption of "EM+ on the "ydro*yapatitie crystals, thereby protecting them from dissolution conditioning solution +ddition of % 7= >*alate to ( 4= nitric acid caused permeability to drop below the initial smear layer value when application times of ,&/%&seconds were
57

!ermeability has also been

shown to decrease when aluminium or ferric o*alate is added to nitric acid

used

+n initial increase in permeability was followed by a marked decrease,

presumably due to precipitation of aluminium or ferric phosphate and calcium o*alate in the tubules The Tenure conditioner, having only ( 4= aluminium o*alate was not as effective in reducing permeability : E Causton et al , ;1872< showed that a ten/ minute application of )TS minerali9ing solution over dentin, improved the performance of ,5= phosphoric acid as adhesion promoters in combination with 1!0/0M+ ;1/phenylglycine with glycidyl methacrylate< a chelating primer "osada et al and Sauk et al ;1878< reported that when new generation clearfil liner bond system was used, in which they treat the dentin with 1&= citric acid containing (&= calcium chloride This high concentration of calcium present may stabili9e collagen during surface etching, but it may also decrease the e*tent of deminerali9ation of hydro*yapatite by a common ion effect 0iscosit( The viscosity of the solutions used to etch has a significant effect on the amount of deminerali9ation Many etchants are purposely thickened to improve handling and limit their distribution on teeth "owever, free diffusion slows down as viscosity is increased so that gets re3uire more etching time than li3uids or stated another way, gels etch dentin less than do li3uids of The same acid concentration and etching time ;Takahashi Su9uki and 1aka, 1881E Erickson 188( < +ccording to study conducted by C F 0uba ;1882<, when three enchants of different viscosities were compared under the scanning electron microscope, the li3uid and thin gel produced a more even etch pattern than a thick gel )n addition the thin gel appeared to produce the most well defined pattern of three conditioners The highest mean tensile bond strength was recorded by the thin gel phosphoric acid ;(&5 (P4( 7kg Jcm(< The li3uid phosphoric acid group etched for 1& secs had the lowest tensile bond strength ;14& ,,2% , kgJcm (< The primary advantage of using a gel is that it gives better control of the acid solution when etching several teeth, and other difficult to reach places :rannstrom, 1ordnwall

58

;1855<

Morphological studies have shown no significant differences based on the

viscosity of the etchant Molecular .ei$#t +n other important variable is the molecular weight or si9e of the etchant, since diffusion varies inversely with the molecular weight Bhile this does not vary much for many acids ;molecular weightsG nitric acid, %,G phosphoric acid 87E citric acid, 18(< )t is more significant with polyacrylic acids, which can have molecular weights that vary from 4&&& to (4 &&& or higher, which decreases their diffusion coefficients )f they also were viscous, then both effects would summate to limit their etching effects Smear la(er Smear tubules ;!ashley and others, 1877aE 6an Meerbeck and others, 188(< Their length ;(/% Mm< is much longer than the thickness of the smear layer )t is the smear plugs that are responsible for most of the reduction in dentin permeability :rannstrom, 1ordenvall and 0lant9 ;187&< advocated treatment of dentin with dilute ;& (=< EDT+ to remove the smear layer without removing the smear plugs This can be accomplished, but the smear plugs will prevent adhesive resin penetration into the tubules ;"amlin, Samarawickrama and -ynch 188&b< ?nder some conditions this might be desirable, while in others it may lower bond strength below what might have been achieved had the resin both penetrated and bonded to peritubular dentin "owever, :ergenholit9 ;187(< consideration on this view is 3uestionable, since solitary microorganisms in particulars anaerobes, with high demands for proper growth conditions, would probably not survive and or multiply on the dentin floor where the nutritional supply is poor and where the microorganisms would be e*posed to host defense factors in the fluids of the dentinal tubules )n general, most materials
7&

are to*ic and bactericidal when they are prepared fresh but lose their antibacterial effects as they cure and age ;"ensten $ !ettersen, 1875, 187% Meryon, 1877< )n the first few days, amalgam and silicate cement are as antimicrobial as 9inc o*ide eugenol, but the antibacterial effects of 9inc o*ide eugenol last much longer ;Tobias, 1877< >riginally, the following of the :rannstrom concept placed great emphasis on the presence or absence of microorganisms in the smear layer 1ovrdenvall, :rannstrom and Torstenson ;1858< predicted that if one microorganism was left in the smear layer, over 1&& billion organisms cloud develop within (2 hours if the conditions were favorable

"owever, :ergenholit9 ;187(< consideration on this view is 3uestionable, since solitary microorganisms in particulars anaerobes, with high demands for proper growth conditions, would probably not survive and or multiply on the dentin floor where the nutritional supply is poor and where the microorganisms would be e*posed to host defense factors in the fluids of the dentinal tubules Conse3uences of remo/al of smear la(er + ma.or problem associated with etching dentin is the increased wetness that results when the smear layer is removed :rannstrom and 1ordenvall ;1855< have presented evidence indicating that the dentin surface becomes decreases the ability of hydrophobic resins to wet such surface, leading too poor adhesion #ecently, this problem has been partially solved by using hydrophilic resins such as "EM+ in concentrations ranging from ,4 to 44= ;Scotchbond (, 0luma<, giving higher dentin bond strengths These higher bond strengths are possible, because these systems remove the limitations of the smear layer by acid etching ;maleic acid in Scotch bond (< or chelation etching ;& 4M EDT+ in 0luma< of the surface )f used properly, these agents remove the smear layer and increase bond strengths, but they also increase dentin permeability
71

This raises the 3uestion of the to*icity of etching agents to the pulp "amin, -ynch and Sarnarawickarama ;188>< in a vitro study demonstrated that the application of a solution of aluminum nitrate and o*alic acid for five seconds was all that was needed to remove Smear plugs

Ferric o1alate use! to !issol/e smear la(er :owen, Cobb and #apson ;187(< introduced the mordanting acidified ferric o*alate techni3ue subse3uently replaced by aluminum o*alate, which dissolved the original smear layer and smear layer Stanley, :owen and Cobb ;1872< and :owen and others ;1878< found very little pulpal responses, due to the blocking of the dentinal tubules with the new artificial smear layer :losser # - ;1875< indicated that the use of purified ferric o*alate solution is ineffective in removing the smeared surface material from either dentin or enamel The removal of this smeared surface layer, previously associated with ferric o*alate solution, was apparently due to the presence of residual nitric acid from the commercial synthesis of ferric o*alate powder :losser and :owen ;1877< and :losser and others ;1878< also found that solutions of aluminum nitrate ;( 4=< and o*alic acid ;1 4=< or .ust ( 2= nitric acid and 4 5= 1!0 ;1/phenly glycine< applied for %& seconds were e3ual effective conditioning agents without the ferric or aluminum o*alate Formation of insolu-le precipitates +nother approach in avoiding the intrinsic weakness of the smear layer ;!ashley 1881< is to remove it, but use some of the mineral in the smear layer to react with ions in the etchant to form insoluble precipitates that adhere to each other and to the underlying dentin matri* more firmly than did the original smear layer particles +n e*ample of that approach was the use of ferric o*alate, in an acid environment, could form insoluble crystals of ferric phosphate ;Eick 188(<, calcium o*alate, and
7(

several forms of calcium phosphate deminerali9ation step

)t is interesting to speculate that the ferric or

aluminum ions may also stabili9e dentin collagen or other macromolecules during the +rguing against that notion is the observation that dentin collagen e*posed during the conditioning step in the Mirage ;Chamelon Dental products< bonding system ;( 4= nitric acid containing 2= 1/phenylglycine< retains its cross/banding This suggests that it is not denatured by acid treatment "owever, some laboratories report relatively low bond strength with this system and claim that the bond fails at the dentin/resin interface Smear plu$s :rannstrom and Fohnson ;1852< noticed that they could remove most of the smear layer but leave the smear plugs in the tubules when they initially scrubbed the surface for five seconds with microbicidal fluoride solutions and then left it for a remaining %& seconds ;')0 27< Result of remo/al of smear plu$s #emoval of the smear plugs by acidic conditioners may result in dentinal fluid flowing from the tubules onto the dentin surface, and this can interfere with the adhesion process )n vitro stimulation of fluid flow to the surface has shown that adhesion is adversely affected by increased permeability Effect of presence of surface moisture +lso 3uantitative measurements of surface moisture have demonstrated that adhesion can be significantly reduced by very small amounts of water on the surface This moisture does not necessarily have to come from the dentinal tubules but could be due to inade3uate drying of the tooth surface after application of a water/based primer Bhatever the source, physisorption of an adhesion promoter can be disrupted by small amounts of moisture and this would affect the ability of bonding agent to wet the surface

7,

Con!itioners On T#e Dentin Surface

The concentrations of acids should be lowered to levels that are isotonic ;appro*imately 1=< with body fluids The etching times should be limited to that re3uired to produce optimum bonding )deally, the depth of etching should not e*ceed 1/( Mm, should not denature collagen, and should leave residual remnants of smear plugs in the tubules to maintain dentin permeability at a low level The chemical effects of conditioners are generally limited to the top 4 m of dentin and, in some cases, to the top & 1 m of the surface The study of these

chemical changes is best/done using surface analysis techni3ues, using */ray photoelectron spectroscopy, recently reported that the elemental composition of fractured dentin and that of smear layer/covered dentin were very similar application of ,= "(>( to smear layers produced no detectable effects The Bhen

Scotchbond Dual Cure adhesive was allowed to react with the smear layer for two minutes, it produced surface deminerali9ationCs that were limited to the outer & &4 mm of the smear layer Treatment of dentin with acids severely depleted the surface of calcium and phosphate +ll these conditioners reduced the surface concentration of calcium and phosphate 'urther, the surfaces became enriched with alcohol groups when treated with Scotchprep ;"EM+<, carbonyl groups with Tenure Conditioner ;o*alate<, and carbo*yl groups when treated with 0luma Cleanser ;EDT+< 'urther, they found no aluminum remaining on the surface after treatment with Tenure Conditioner ;aluminum o*alate< Most importantly, since */ray photoelectron spectroscopy provides information about the binding energies of various chemical groups, they found no evidence of any shifts in binding energies of reactive groups on dentin that would signal the development of primary bonding The treatment of dentin with acidic conditioners leaves the surface so depleted of calcium and enriched by organic residues that subse3uently placed bonding systems should be based upon agents able to interact with the organic components of dentin :onding agents that rely on chelation to calcium are unlikely to be successful when applied to acid/etched dentin unless they penetrate into the deminerali9ed matri* to reach normal minerali9ed dentin

72

O/ray photoelectron spectroscopy ;O!S< combined with secondary ion mass spectrometry ;S)MS< is very useful in the study of the effects of conditioner treatments on dentin surface The use of ion beams to erode the surface under controlled conditions permits depth/profile analyses to be made Energy/dispersive */ ray spectroscopy ;EDS< lacks the ability to restrict the analysis to the surface, as if penetrates several micrometers into the surface "owever, it has the advantage of high/resolution ;spot si9e<, and it can provide maps of the distribution of elements 1one of these surface analytical techni3ues can determine whetherE the tertiary structure of collagen is normal or how well resins have wetted dentin surfaces Thus, transmission and scanning electron microscopy remain important research tools in this area The concentration of acids used to etch dentin is evolving to lower concentrations than the initial ,5= phosphoric acid concentration ;'usayama1872< :isco now uses 1&= phosphoric acid in their +ll/Etch techni3ue Tenure and Mirage :ond both use ( 4= nitric acid treatment This procedure was shown to be without significant pulpal response in e*perimental animals Fust as investigators have recently recommended shorter etching times and lower concentrations of acids for enamel, and recently recommended shorter etching times for dentin conditioners )f reductions in acid concentration and etching time do not lead to a decrement in bond strength, then they should be employed :owen has long advocated the use of isotonic acid solutions to avoid osmotic insult to odontoblasts

%IOCOM ATI%ILITY
Since the mid 184&s, a number of publication have reported that etching of vital dentin will cause pulp inflammation and eventual necrosis ;Lramer and Mc-ean, 184(E 'ran3uin and :roulliet 1877< !rofessor 'usayama ;1875< reported that in vivo etching of dentin and proper sealing of the dentinal tubule and 'usayamau187(E 'u.initi 187%< have demonstrated that direct application of various etchants to vital dentin and subse3uent treatment with their compatible adhesive systems provided a seal against microleakage 1o pulpal response was recorded when these etchants and bonding materials were evaluated for international biocompatibility testing
74

+ recent study of a vital acid etching system ;Bhite and >thers 188(< employing 1&= phosphoric acid treatment placement onto vital dentin of freshly prepared on non human primate teeth demonstrated no pulpal inflammation or bacterial leakage after (4 and 7& days as per )S>, 'D) and +D+ testing criteria for usage evaluation Most of the recent generation of dentin bonding agents has recommended removal of the outer contiguous smear layer as well as well as all or portions of underlying smear plugs Bith the advent of enamel$dentin etch ants that may disinfect the remaining affected dentin, as well as the newer hydrophilic primer and bonding system that infiltrate into the dentin substrate, our clinical profession may e*pect to place adhesive and composite systems that are biologically compatible with the dentin and pulp )n addition, these newer systems provide a durable bonding and hybrid mechanism to the tooth structure that should be e*pected to continuously prevent microleakage of bacterial contaminants )t has been suggested that conditioning agents ;etching agents used on dentin< should beG )sotonic to avoid osmotic pressure changes in dentinal tubules >f neutral p" or at least between p" 4 4 and p" 7 &E 1onto*ic to dentin, pulp and gingival tissue Compatible with the chemistry of the materials it will contact Bater soluble and easily removed ?nable to deplete the enamel or dentin chemically +ble to enhance the surface chemically in preparation for bonding )mportant variables regulating the type of pulpal response to etched dentin The type of acid, pLa and p" +pplied concentration ;which determines its chemical potential and osmotic pressure< The time of etching ;acid challenge R time O concentration< #emaining dentin thickness ;SP& %mmT<
7%

The ability of subse3uently placed restorative materials to seal dentin pH Many dentin conditioning agents have p" values much lower than 4 4 +cids can challenge pulp vitality no matter what the source, and they can harm the pulp if they approach or contact it The smear layer and tubular plugs ;the smear unit< and per tubular dentin ;sclerotic dentin< can be rapidly dissolved by strong acidic conditioning agents when applied for e*cessive ;e*tended< time intervals ;Mount, 188&E !ashley and Depew, 187%E !ashley, 1877E !ashley and others, 1877E Stanley, 188&<

ulpal reactions !epen!in$ on p# Cytoto*ic effects within the pulp tissues can be caused by low p" hypertonic and hypotonic concentrations ;abnormal osmolality<, or chemical interferences with vital biochemical reactions ;M.or, "ensten $ !ettersen and :owen, Fohnson and others 185&< Concentration of aci! The concentration of acids used to etch dentin is evolving to lower concentrations than the initial ,5= phosphoric acid concentration ;"osoda and 'usayama, 1872< :isco now uses 1&= phosphoric acid in their +ll Etch techni3ue Tenure and Mirage :ond both use ( 4= nitric acid treatment This procedure was shown to be without significant pulpal response in e*perimental animals ;:losser and others, 1878< Fust as investigators have recently recommended shorter etching times and lower concentrations of acids for enamel times ;:astos and others, 1877E -egler and others, 1878<, :losser ;188&< recently recommended shorter etching times for dentin conditioners )f reductions in acid concentration and etching time do not lead to a decrement in bond strength, then they should be employed
75

The concentration of an acid reaching the pulp tissue is determined by how much penetrates through dentinal tubules and reaches along the way with hydro*yapatite and proteins contained within the tubules The absolute concentration of an acid is reduced over distance such that at relatively large thickness ;T1 & mm< the concentration of a substance is relatively low by the time it reaches the pulpal surface

+s the remaining dentin thickness decreases, there is less recognition of solute concentration, causing a meager concentration at the pulpal surface as the diffusing solutes reach the end of the tubules ;!ashley, 1858E !ashley, 1874 and >thers< Contributing to the immediate pulpal irritation of acid etching is the fact that in etchants are very hypertonic and tends to osmotically draw fluid from the pulp to etchants ;Macko and >thers, 1857< +cidic solutions can and do denature proteins including collagen, non/collagenous proteins, en9ymes in odontoblastic processes Thus, the acidity and hypertonicity of acidic conditions should cause an immediate pulpal reaction +s protons are buffered by the trivalent phosphate of hydro*yapatite, the mono and divalent forms of phosphate no longer fit the crystalline lattice structure of hydro*yapatite and it disintegrates These changes in dentin are readily seen in Scanning Electron Micrograph ;SEM< e*aminations of fractured surfaces of acid etched dentin/ The funneling of the top of dentinal tubules due to the dissolution of peritubular dentin provides physical evidence of the depth of penetration of hydrogen ions during the brief ;,&/%& seconds< etching periods used clinically The loss of peritubular dentin mineral is more dramatic than that of intertubular dentin, because it contains little collagen and thus disappears when it is deminerali9ed The same buffering of hydrogen occurs in intertubular dentin, but because of its high collagen content There is little loss of substance that can be seen by Scanning Electron Micrograph
77

" # Stanley et al ;1854< reported that 4&= citric acid or phosphoric acid is detrimental to pulp when placed over dentin The intensity of pulp response to composite was increased after acid pretreatment of the dentin )t was also suggested that when the remaining dentin thickness was one mm or less than that, the area had to be protected, even when a composite of neutral ph containing no methacrylic acid was used !erdiago et al ;188%< studied the effect of si* phosphoric acid etching agents and depth of deminerali9ation human dentin under scanning electron microscope The results obtained suggest that similar concentrations of phosphoric acid etchants containing distinct thickness result in different deminerali9ation 1umerous investigators have reported that acid etching of dentin leads to pulpal inflammation Several in vitro studies indicated that dentin restricts the penetration of hydrogen ions Their results indicate that brief e*posures to acid lead to little penetration of hydrogen ions across dentin that is & 2 to & 4 mm thick This is due, in part, to the e*cellent buffer capacity of dentin The calculated depth of penetration of a small acid such as nitric acid into dentin in 2& seconds is 78 Mm :losser ;188&< recently reported that ( 4= nitric acid funneled the orifices of dentin to a depth of 4Mm in 2& seconds 'unneling of tubule orifices provides physical evidence of the depth of penetration of protons into dentin "ol9Cs group ;Cotting and >thers 187&< also found the acid etching of human dentin in vivo with ,5= phosphoric acid produced only a mild pulpal response if the etched dentin was subse3uently covered with calcium hydro*ide )f it was covered with calcium hydro*ide first and then acid etched, there was more severe pulp response due, in part, to the greater loss of the bases during acid treatment

Etching techni3ues that utili9e a high concentration of acid with a low p" and a long interval of application ;%& $ 1(& seconds< when loosely appro*imating the pulp can intensify the pulpal response with neutrophilic infiltration -ocal tissues in.ury
78

that damages small vessels causes leakages of plasma containing fibrinogen and fibronectin The e*travasated fibrinogen becomes clotted and cross/linked to trap migrating neutrophils 1eutrophils arrive first at the site of in.ury not only due to their mobility, but because they are also chemo attracted by the fibronectin 1eutrophils then produce their own chemo/attractants that induce the migration of additional occur with 9inc o*ide eugenol Therefore, it is unlikely that the influ* of neutrophils following dentin conditioning techni3ues is due to increased permeability of the dentin and the increased ability for the eugenol to reach the pulp, it appears that certain conditioning agents can of themselves causes or intensify pulpal responses Reco/er( of pulp Bithin (2 / 27 hours the pulp should recover from these sterile insults, as the tubules should be sealed by adhesive resin films )f one observes pulpal irritation beyond three days, then one should suspect that there is some continual source of irritation that has nothing to do directly with the acid used to etch the dentin or the subse3uently placed resin, because most of the reachable products from such resins diminish rapidly over time ;"ume and Mount 1877E "anks and others 1877< -ikely candidates for such irritation are bacteria and their products, which gain access to the cavity walls because the restoration did not seal the dentin well 0erm/free studies indicate that pulps heal rapidly even when bonding agents are placed directly on the pulp ;)noue and Shimono, )88(< Duration of aci! e1posure into a smear la(er )t is useful to calculate how many seconds of acid e*posure are re3uired to allow the acid to penetrate 1mm into a smear layer surface ;the thickness of an average smear layer< )f one assumes that the acid has a diffusion coefficient of 1 O 1&/% cm(Jsec, the diffusion time is only five milliseconds +ssuming a 1&/fold lower effective diffusion coefficient ;which may be the case for higher molecular weight polyacrylic acids gels< e*tends the time to & 4 seconds Thus, it appears that the
8&

etching times that have been used are more than those re3uired to diffuse through the smear layer C#emical effects of con!itioners The chemical effects of conditioners are generally limited to the top 4 m of dentin surface ;#use and Smith, 1881< ?sing */ray photoelectron spectroscopy, recently reported that the elemental composition of fractured dentin and that of smear layer/ covered dentin were very similar They found that application of ,= hydrogen pero*ide to smear layer produced no detectable effects Difference in reaction of toot# accor!in$ to a$e The pulp of younger virgin tooth with open dentinal tubules to begin with is more susceptible to the to*ic components of dental materials and responds with more intense inflammatory reactions than does an older tooth, which over the years has produced a considerable amount of sclerotic dentin, and reparative dentin that blocks the tubules Sure attempts to protect the pulp with ;a< sclerosis of dentin, either as a natural process of aging or induced by the irritation from caries, attrition, abrasion and erosionE and b< reparative dentin formation, induced by the above restorative factors and also by tooth cutting and restorative proceduresE Stanley and others, 187&<

0ARIOUS ACID CONDITIONERS #osp#oric aci!

The 'ist Dentin Conditioner phosphoric acid li3uid removes some surface dentin and leaves a clean, well $defined etching pattern The tubule orifices are enlarged into a funnel shape !hosphoric acid gels, thickened with fumed silica, similarly open the tubules but also leave a substantial covering of the thickening agent on the dentin #egardless of e*tensive washing, the silica is not entirely removed 'usyama and >thers ;1858< were the first to report the successful use of phosphoric acid to remove the smear layer, etch the dentin and restore with adhesive composite resin 'or some years there was an unresolved discrepancy between clinical
81

success and etched dentin ;Shintani, Sataou and Satou, 1878< and research that seemed to contraindicate phosphoric acid etched dentin #ecently Lanca reevaluated the literature "is concluding hypothesis was that eugenol, not phosphoric acid, most likely led to pulpal irritation, as previously thought to be associated with phosphoric acid )t was the first dentin conditioner that was successfully used to remove the smear layer etches the dentin and restore with adhesive composite resin by 'usayama and >thers ;1858< This helps in removing the surface dentin, leaving a clean wee defined etching pattern where the tubules are enlarged into funnel shaped !hosphoric acid is the acid of choice currently for the etching purpose concentrations in clinical practice e*ceed ,&= phosphoric acid "owever controversy remains about the optimal concentration of phosphoric acid The most widely used

Nitric aci! )t is stronger than phosphoric acid, it easily removes the smear layer ?sed in concentration of ( 4= causes funneling of the orifices of dentin to a depth of 4M in 2& seconds 1itric acid conditioners are highly adhesive and provide good tubule seals Citric aci! 1&= citric acid is used for the purpose of removing the smear layer )t has been reported by 1akabayashi ;1878< that such treatment tends to lower the porosity or permeability of the deminerali9ed surface, possibly by denaturing the collagen 1&= citric acid plus ,= ferric chloride and the combination was developed by 1akabayashi The divalent caution seems to stabili9e the dentin matri* during its deminerali9ation by citric acid This combination was found to be particularly effective for methacrylate based adhesives containing 2/MET+ Several Fapanese products remove the smear layer with 1&=citric acid 1akabayashi ;1878< has reported that such treatment tends to lower the porosity or permeability of the deminerali9ed surface, possibly by denaturing the collagen "e
8(

developed 1&/, solution ;1&= citric acid plus ,= ferric chloride<, in which the divalent cation seems to stabili9e the dentin matri* during its deminerali9ation by citric acid The higher bond strengths of 2/metharylo*yethyl trimellitic anhydride J methylmethacrylate/tetrabutyl borane o*idi9ed comple* failed to produce pulpal inflammation or necrosis

(ru/ic aci! !yruvic acid and pyruvic acid buffered with glycine have been reported to satisfactorily acid etch both enamel and dentin ;+smussen and Munksgaard, 1877< when using the 0luma bonding system 0lycine was used to ad.ust the p" and perhaps to facilitate polymeri9ation reactions Lactic aci! The study conducted by +yad M ' et al ;188%< revealed that lactic acid dissolved the smear layer with various degrees of etching and deminerali9ation The degree of smear layer and matri* removal was proportional to the concentration of the acid and the length of application time + (&= lactic acid concentration applied for 1&secs produced a clearly etched surface with minimal deminerali9ation + ,&= concentration not only removed the smear layer and enlarged the dentin tubule orifices but also appeared to affect the collagen matri* ol(acr(lic aci! !olyacrylic acid is effective in removing the smear layer and is commercially available in products such as Clearfil Tooth cleanser ;Dents ply -td< that contains (4= phosphoric acid and is marketed as a cavity conditioner for glass polyalkeonate restorative materials for 1& seconds NaOcl as a !entin con!itioner

8,

The manufacturers of Dentin +dhesit ;6ivadent, Tonaeanda, 1I 1214&< included a solution of 4= 1a>cl as a dentin conditioner This was designed to solubili9e the denatured collagen that had become gelatini9ed on the surface +s this treatment did not change the permeability of smear layer covered dentin ;!ashley, unpublished observation<, many thought that such treatment was without effect "owever, recently published transmission electron microscopy of 1a>cl / treated smear layers revealed that the agent penetrated 4/1& mm below the smear layer )t also seemed to alter the subsurface dentin matri* in a subtle manner The functional significance of this is unknown The observation emphasi9es the conse3uences of attempting to modify the surface of a smear layer 1/(mm thick These agents easily diffuse through the smear layer in a few seconds and may produce undesirable subsurface effects C#elators EDTA Contrary to the use of strong acid etchants, chelators are used to remove the smear layer without decalcification or significant physical changes to the underlying substrate The best known chelating conditioner is ethylenediamine tetra acetic acid ;EDT+< ad.usted to !" of about 5 2 )t was developed for use in the 0luma ;Miles, )1C, Sout11 1874< Bhile the smear layer is removed, no significant surface concavity is formed and the funnel shape changes associated with phosphoric acid is not evident :rannstromCs concerns that bacteria might be incorporated into smear layers and infect the dentin surfaces of cavities led him to develop a dentin conditioner containing & (= ethylene diamine tetraacetic acid, ;EDT+, p" 5 2< and & 1= ben9alkonium chloride as a surface/active disinfectant 1ordenvall and 0lant9, 187&E :rannstrom and >thers, 187(< This agent, marketed under the name Tubulicid ;Dental Therapeutics +:, 1acka, Sweden<, is scrubbed on the surface of the smear layer for a few seconds, then
82

;:raannstrom,

left on passively for another %& seconds, followed by additional scrubbing

Such

treatment indeed does remove the smear layer and generally leaves smear plugs intact The permeability of dentin remains low and unchanged by such treatment, although a few areas can be seen where the smear plugs are gone permeability suggests that the latter effect is minor Stagel, >stro and Cesare ;1875< reported that dentin conditioned with Tubulicid increased the bond strength of Scotchbond J Silu* ;,M Dental !roducts< !ashley Tao and ;1877< reported a significant decrease in the shear bond strength of The lack of change in dentin

Scotchbond JSilu* when samples were treated with Tubulicid, although there was no change in dentin permeability ;Tao and !ashley, 1878b< !resumably, the dilute solution of EDT+ removed some surface calcium that is thought to be important in the mechanism of bonding of Scotchbond Dual Cure to dentin This was probably responsible for the fall in bond strength Causton ;1872< reported that Scotchbond Dual Cure gave lower bond strengths to deep dentin compared to superficial dentin "e assumed that this result was due to a lower minerali9ation in deep dentin Topical application of a minerali9ing solution ;Causton, 1872< increased the bond strength of Scotch bond to deep dentin but did not enhance bonds to superficial dentin The use of minerali9ing solutions as dentin To be practical, they should conditioners has not received much further attention produce a significant effect within two minutes

Most of the second/generation dentin bonding agents that did not use dentin primers or conditioners produces bond strength to smear layer/covered dentin of about 4/5 Mpa ;Surmont and >thers, 1878< on e*tracted human dentin Careful scanning electron microscopy e*amination of both sides of the failed bonds revealed smear layer particles on each surface ;!ashley, 1881< This indicated that the 4 Mpa really represented the cohesive strength of the smear layer That is, the bond to the top of the smear layer remained intact and the @bondA of the lower half of the smear layer to the underlying dentin matri* remained intact,
84

but the smear layer had split

Bhen the smear layer was treated with ;4=

0luma ;Miles, )nc, Dental !roducts, South :end, )1 2%%12< !rimer strength Similar results were obtained in vivo ;!ashley and >thers 1877< This is primarily due to improved wetting of the surface

glutaraldehyde in ,4= "EM+<, we obtained a significant increase in shear bond

"owever, it is

possible that the smear layer is falling closer to the dentin surface, where the cohesive strength of the smear layer may be higher >thers have obtained relatively high bond strengths to smear layers Surmont and others ;1878<, using the 0luma bonding system, compared the tensile bond strengths in three different treatment groups The group in which the smear layer was treated with water gave a mean tensile and strength of 1& & S 1 8 M!a The group treated with 1eo/Sabeny J Tubulicid ;which removed the

superficial smear layer but not the smear plugs< had a mean bond strength of 1& 1S ( & M!a The group treated with EDT+ had a lower bond strength ;5 2 S 1 2 M! a< The latter value is similar to what was obtained for 0luma J Scotchbond J Silu*<

The smear plugs in the dentinal tubules are not fully removed by ,& seconds application of the conditioner The system uses both glutaraldehyde and "EM+ in a primer that is applied after the EDT+ conditioner removes the smear layer Maleic aci! Maleic acid ;e g , Scotochbond (, ,M dental products< also results in removal of the smear layer but not the smear plugs +lthough it is acidic it does not appear to decalcify deeply, and the hybrid layer is comparatively thin The thickness of the hybrid layer does not have much effect on the dentin bond strength ;')0 41< :rannstromCs concerns that bacteria might be incorporated into smear layers and infect the dentin surfaces of cavities led him to develop a dentin conditioner containing & (= ethylene diamine tetraacetic acid ;EDT+, p" 5 2< and & 1= ben9alkonium chloride as a surface active disinfectant ;:rannstrom and 1ordenvail
8%

187(<

This agent, marketed under the name Tubulicid ;Dental Therapeutics +:, Such

1acka, Sweden<, is scrubbed on the surface of the smear layer for a few seconds, then left on passively for another %& seconds, followed by additional scrubbing treatment indeed does remove the smear layer and generally leaves smear plugs intact The permeability of dentin remains low and unchanged by such treatment, although a few areas can be seen where the smear plugs are gone The lack of change in dentin permeability suggests that the latter effect is minor bonding of Scotch bond Dual Cure to dentin The dilute solution of EDT+ removed some surface calcium that is thought to be important in the mechanism of

Lasers "ard tissue -+SE#S in dentistry are an emerging technology + pulsed 1dGI+0 laser will not disturb the pulp, even when the approach is as close as 1mm ;Bhite and others 188&< "eat is dissipated between the 1& to ,& pulses per second The mechanism of dentin removal is microscopic e*plosions caused by the thermal transients Bhile most research has been conducted on dry dentin, the laser will operate on dentin immersed in saliva and water The carboni9ed, black soot that results is easily washed off with water The lased surface results if desensiti9ed dentin, presumably by occlusion of the open and permeable dentinal tubules Microorganisms and organic debris are eliminated from the lased surfaces ;Bhite, 0oodis, Cohen 1881< The laser decreases the organic fraction and increases the inorganic fraction of dentin surface ;Bhite and >thers 1881< -asing of the dentin has the potential to increase the bond strength of current dentin bonding agents )ts effect on the bond strength of Scot bond ( was recently presented by Bhite and others ;1881<

85

The bond strength increased about %&= compared to the smear/layered dentin presumably by increasing the bondable inorganic fraction of the dentin surface The laser may create micro mechanical retention, which is an analogue to the effect seen on laser/etched surface +ccording to +rturo Martine9/)nsua et al ;(&&&<, tensile bond strength s of bonded brackets obtained after laser etching were significantly lesser than those obtained with acid etching They also showed that enamel and dentin surfaces prepared with Er/I+0 laser etching showed e*tensive subsurface fissuring that is unfavourable to adhesion Microa--rasion Modification of dentin by micro abrasion is another emerging technology Micro abrasion with aluminium o*ide removes healthy as well as diseased dentin and results in a smear layer The abrasion action of aluminium o*ide depends on the particle si9e as well as on the velocity !articles & 4Mm or less in diameter do not affect the enamel e*cept to cleanse it The & 4/micron or larger particles create a smear layer on the dentin and increase the surface area ;:lake 1881< This smear layer might be used to enhance the bond strengths of smear/mediated dentin bonding agents Uni/ersal con!itioners Several laboratories have attempted to produce @?niversal ConditionersA That is, conditioners that remove the smear layers from both enamel and dentin in a single treatment Most dentin conditioners ;for e*ample, 1&/, solution< do not ade3uately etch enamel in ,& seconds Thus it would save time and simplify the techni3ue, if a single treatment could etch both surfaces
87

SELF&ETCHIN" RIMER
Self/etching primers can provide an effective alternative to conventional phosphoric acid etchant in conditioning the enamel surface to secure a durable bonding and marginal seal of composite resin restorations Self/etching primer adhesive systems are characteri9ed by the simultaneous deminerali9ation of tooth surfaces and monomer diffusion into tooth substances Contemporary self/etching primers and the recently introduced all in one adhesive are attractive additions to the clinicians bonding armamentarium They are user friendly in that the number of steps re3uired in the bonding protocol is reduced +s the smear plugs are not removed prior to the application of these adhesives, the potential for post$operative sensitivity that is caused by incomplete resin infiltration of patent dentinal tubules can be substantially reduced More over, as water is an essential component of these systems to enable ioni9ation of the acidic monomers for deminerali9ation of hard dental tissues, the techni3ue sensitivity associated with variations in the state of hybridi9ation of a deminerali9ed collagen matri* is also eliminated Due to itCs intrinsic acidity, the self $etching primer dissolves the enamel surface and thereby creates a three dimensional micro retentive surface pattern, while simultaneously promoting monomer infiltration Depth off enamel deminerali9ation and penetration depth of bonding agents are therefore identical, since both processes run parallel to each other +s a result, light curing of these interpenetrated monomers and copolymerisation with the over lying resin bonding agent and composite resin form a continuous bond with the enamel surface capable of resisting the effect of micro leakage
88

Since the primer is not rinsed after application, but air/dried only, the calcium and phosphate ions that were dissolved from the hydro*yapatite crystals must be suspended in the watery solution of the primer Bhen the water is evaporated during air/drying, the concentrations of solubili9ed calcium and phosphate salts within the primer may e*ceed the solubility product constants for the number of calcium phosphate salts !resumably, minerals will then precipitate within the primer These high concentrations of calcium phosphate will tend to limit further dissolution of the apatite due to common ion effects of calcium and phosphate and thereby limit the depth of enamel surface deminerali9ation >n the other hand, it is very likely that the binding of calcium ions to the phosphate residues in the primer molecules contribute to the inactivation of molecules acidity )n addition, evaporation of water during air drying, as well as light curing of the primer and subse3uently applied bonding agents, and restrict and inhibit the self etching effect of primer molecules 'or adhesion to dentin, all self/etching primers dissolved the smear layer and caused better infiltration of hydrophilic monomer into dentin to create a hybrid layer +nother reason for better marginal sealing may be improvement in the mechanical properties of bonding resins )t has been suggested that improvement of the mechanical strength of the bonding resin leads to an enhancement of bond strength M "anning et al ;1888< in their article concluded that self etching primer can provide an effective alternative to conventional !hosphoric acid etchant in conditioning the enamel surface to secure a durable bonding and marginal seal of composite resin restoration, tested on bovine enamel +ccording to Shahabi et al ;1885<, the shear bond strengths in the order of 1& Mpa can be obtained reliably on human teeth using laser conditioning with pulsed modes in the absence of any other preparation of the natural enamel surface

1&&

Miyasaka L ;1888< showed that high 3uality hybridi9ation was possible by combining EDT+ conditioner and phenyl/!J"EM+ self/etching primer bonding system was promising for bonding resin to human dentin This

EFFECT OF ETCHIN" ON RIMARY TEETH

Silverstone ;1852< found that a %&sec application of an unbuffered solution of ,5= phosphoric acid produced the most favorable conditions for bonding 'ukes et al ;1872< and Eidelman et al ;1872< showed, respectively, that a (& sec etch provided similar leakage resistance and retention rates when compared to a %& sec etch This has very obvious implications for the management of young children when scaling
1&1

their teeth and therefore upon the success of the sealant itself +cid etching has two distinct actions on human enamel Firstly, it removes superficial pla3ue, debris and a very shallow layer of enamel, including chemically inert enamel crystallites Secondly, it renders the enamel surface more porous + honey/combed latticework is produced within the remaining superficial enamel, where enamel tags are left pro.ecting in different planes and at different angles There is differential deminerali9ation of the prisms because the primary attack occurs on the cores of enamel rods to produce the microspaces "owever, this depends on the incident angulation of the enamel rods to the tooth surface >n an average, the etching is about (4Mm deep in permanent teeth )t was thought the outer prism less layer of primary enamel ;#ipa 18%%<, prevented the penetration of resins in the surface of etched primary enamel ;Sheykholeslam an :unocore 185(< There is no universal agreement that prism less enamel occurs in all surfaces of all primary teeth ;Mortimer185&E Silverstone 185&< To obtain a pattern of etching comparable to that found in permanent teeth, Silverstone and Dogan ;185%< found it necessary to etch for 1(& seconds "owever, #edford et al ;187%< looked at the effect of different etch times on the sealant bond strength, etch depth and pattern, on primary teeth They found that the bond strength was no greater at %& or 1(& seconds than at 14 or ,& seconds, but the standard deviation was greater at the two shorter timesE the etch depth was not very different at the three shorter times but was five times greater at 1(& seconds They felt unable to recommend an etch time for primary enamel of less than %& second because of the greater variability of bond strength at 14 and (& seconds >ur clinical e*perience is of good results with a ,& second etch

1&(

LICATIONS OF THE ACID CONDITIONERS

+cid etch techni3ue is now widely used for most composite restorations as a

means of aiding retention and reducing or preventing micro leakage choice for restoring the tooth contours and function

'or class/2

cavities the acid etches techni3ue has replaced the gold inlay as the treatment of

:onding of resins using the acid etch techni3ue has also been used as a means of splinting teeth which have been weakened by cavity preparation 'issure sealants are now widely used for preventing pit and fissure caries #esin systems are now used for attaching orthodontic brackets Composites are gaining in popularity for the attachment of bridges The principle of the resin/bonded system is that the composite bonds mechanically to the etched enamel of the tooth and also to the surface of the cast alloy framework of the bridge

1&,

+nother application of the acid etch techni3ue is the attachment of acrylic or porcelain labial veneers in order to improve the appearance of stained, discolored or misshapened teeth +ll in all, the accumulating knowledge indicates that since only the surface of the dentin, needs to be modified and not its depth, conditioning techni3ues that utili9e weaker acids, shorter periods of applications, and the elimination of rubbing and scrubbing procedures perform 3uite satisfactory and produce minimal pulpal responses #upp ;1871< %= citric acid, 14 secondsE +-/1ahedh and >thers ;188&<

DISAD0ANTA"ES OF ACID CONDITIONERS

There are a number of disadvantages to acid etching of dentin These includeG )ncreasing dentin permeability )ncreasing dentin wetness )ncreasing the potential for pulpal irritation by leakage of microbial products )ncreased potential for denaturation of collagen andJor reducing the porosity of the deminerali9ed matri* by precipitation of calcium and phosphate ions There is also the danger that adhesive resins will not penetrate into the matri* as deeply as the acidic conditioners This may leave an intrinsically weak 9one that may give high bond strengths initially, but weaken over several years due to slow hydrolysis of e*posed, unprotected collagen

1&2

FACTORS TA:EN INTO CONSIDERATION

Bhen evaluating whether an etching techni3ue is good or bad, one must remember that subtle changes in techni3ue and methods can cause important changes in results, and that the following factors must be taken into considerationG Type of acid Concentration Time interval of applicationE +ctive ;rubbing, scrubbing< or passive ;soaking< application Cavity preparation or .ust e*posed superficial dentin Consideration of #emaining Dentin Thickness ;#DT< !resence or absence of sclerotic dentin and reparative dentin +ge of the patient and species and age of e*perimental dentin !ulpal responses to subse3uent type of restoration o Condensation of amalgam
1&4

o Self $cured composite resin, placed under pressure o 6isible $ light cured composite resin placed incrementallyE and !ulpal response to a fresh mi* of restorative materials or to a cured disc of the material in 3uestion placed in a leaching solution to measure the release of "S

ACID

CONDITIONERS

FOR

"LASS

IONOMER

CEMENTS
"lass Ionomer Cements -ike most etching procedures, acid etching of dentin before placement of glass / ionomer cements has evolved from relatively harsh treatment ;2&= polyacrylic acid for ,&/%& seconds< to relatively mild treatment ;1&= !olyacrylic acid for 14 seconds, !owis and >thers 187(E :erry, 6on der -ehr and "errin 1875< 'ew investigators have defined the purpose of what this etching was designed to accomplish other than to increase the bond strength of glass/ionomer cement to dentin !resumably, they were attempting to remove the loose particles that make up the smear layer from the surface to permit interaction of the glass/ionomer cement with the underlying surface "owever, as conventional glass/ionomer cement seems to interact with surface calcium ;Bilson and Mclean 1877<, it would appear that any acid etching that is sufficient to remove the smear layer would deplete the surface of calcium and interfere with subse3uent surface reactions )ndeed, careful e*amination of the literature revels as many reports of acid etching having no effect at increasing glass/ ionomer cement bond strength as those that show an increase

1&%

SURFACE CONDITIONS +dhesion to dentin is enhanced by surface conditioning with (4= solution of polyacrylic acid for 1& seconds 0lass/ionomer cements, being polar substances, are capable of ion/e*change with the tooth structure, and they have similar thermal e*pansion to enamel and dentin and also very low shrinkage on setting :y contrast dentin bonding agents used with composite resins, although showing higher initial bond strengths, generally deteriorate under stress caused by fle*ure of the tooth, polymeri9ation shrinkage or hydrolytic in stability ;Bilson and Mc-ean 1877<

1&5

%I%LIO"RA HY
+ - 1ahedh, " 1 !hilips, # B Cochran M C and Swart9 M - ;188&< Efficacy of selected smear layer removing agentsG + SEM study Fournal of Dental #esearch %8 +bstracts of !apers 1(7 +bstract 147 +nusavice !hilips Science of dental materials O Edition B : Saunders Company ! ,&2/,&5 +rturo Mantine9 $ )nsua, -uis da Silva Domingue9 ;(&&&< Differences in bonding to acid etched or ErGI+0 laser treated enamel and dentin surfaces Fournal of !rosthetic Dentistry 72, (7&/(77 +smussen E and Munksgaard E C ;1874< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/ 82 +smussen E and Munksgaard, e c ;1874< +dhesion of restorative resins to dentinal issues in !osterior Composite #esin Dental #estorative Materials eds 6anheds 0 and Smith D C pp (15/((& +smussen E and Munksgaard E C ;1874< :onding of restorative resins to dentine promoted by a3ueous mi*tures of aldehydes and active monomers )nternational Dental Fournal ,4G 1%&/1%4

1&7

+smussen M and :owen # - ;1875< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/82 +yad M ' , #osenstial S ' , 'rag + M ;188%< + pilot study of lactic acid as an enamel and dentin conditioner for dentin bonding agent development !rosthetic Dentistry 5%G (42/(48 ;+bstract !apers< :ates D , #etief D " , Famison " C ;187(< cited $ Clinical application of enamel adhesives by D " #etief >perative Dentistry, Supplement 4G 188(E 22/28 Fournal of

:astos ! , #etief D " , :radlet E - ;1877< cited $ )nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4G 188(E 1,5/14& :enderli I , Iucel T ;1888< The effect of surface treatment on the bond strength of resin composite to dentin >perative Dentistry (2G 8%/1&( :enediktson S ;1881< cited $ # - Erickson, Surface interactions of dentin adhesive materials >perative Dentistry, Supplement 4G 188(E 71/82 :ergenholti9 0 ;187(< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4G 188(E 141/1%2 :erkovit9 : L : , "olland 0 # , Mo*ham : F + colour atlas and te*tbook of oral

anatomy, histology and embryology Bolfe !ublishing -td :erry E + , 6onder -ehr B 1 ;1875< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& :lake T ;1881< cited $ Conditioning of the dentin substrate by # - :entolotti >perative Dentistry, Supplement 4, 188(, 1,1/1,7

:losser # - , #upp 1 B , Stanley " # and :owen # - ;1875< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&
1&8

:losser # -

:owen # - , ;1877< Effects of purified ferric o*alate J nitric acid

solutions as a pretreatment for the 1T0 $ 0M+ and !MDM bonding system Dental Materials 2, ((4/(,1 :losser # - , :owen # - ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 :losser # - , #upp 1 B , Stanley " # , :owen # - ;1878< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( :losser # - , #upp 1 B , Stanley " # ;1878< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 :losser # - ;188&< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& :owen #- ;18%(< $ cited / Dental filling materials comprising vinp reline treated used silica and % binder consisting of the reaction product of bisphenol + glycidyl acrylate ? S !atent , & 4% 11( :owen # - ;18%4< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2

:owen # - ;1857< +dhesive bonding of various materials to hard tooth discuses solubility of dentinal smear layer in dilute acid buffers )nternational Dental Fournal (7G85/1&5 :owen # - , Cobb E,1 , #apson F E ;187(< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2
11&

:owen # - , Cobb E 1 , Misra D 1 ;1872< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 :oyde + , Switsur 6 # , Steward + D ;18%,< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/ 14& :oyde + ;18%4< The structure of developing mammalian denial enamel )nE Slack M6, 'earnhead #B eds Tooth Enamel, 1%,/5/ Bright :ristol :oyde + ;185%< Enamel structure and cavity margins >perative Dentistry 1,1, 1,/ (7 :oyde + ;1878< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 :rannstrom M , Fohnson 0 ;1852< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2

:rannstrom M , 1ordenvall L F ;1855< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 :rannstrom, M and 1ordenvall, L F ;1855< The effect of acid etching on enamel, dentin, and the inner surface of the resin restorationG a scanning electron microscopic investigation Fournal of Dental #esearch 4% 815/8(, :rannstrom M , 1ordenvall L F ;1855< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( :rannstrom M , 1ordenvall L F , 0lant9 ! > ;187&< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&
111

:rannstrom M , 1ordenvall L F , 0lant9 ! > ;187&< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( :rannstrom ;1871< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 :rannstrom M , 0lant9 ! > , 1ordenvall L F 4, 188( 1,5/14& :rannstrom M ;187(< Dentin and !ulp in #estorative Dentistry, -ondonG Bolfe Medical !ublishers ;187(< cited $)nteractions of

conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement

:rannstrom ;1872< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( :rown et al ;1877< cited / LennedyCs !ediatric >perative Dentistry 2 th Edition Fohn Bright and Sons -td , 188%E %,/55 :uonocore M 0 ;1844< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/15% :uonocore M Bileman B and :rundevold ' ;184%< $ cited / + report on a resin composition capable of bonding to human dentin Surfaces Fournal of Dental #esearch ,4 72%/741 :yers M# ;187&< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 :yers M# ;1872< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15
11(

:yers M# ;188%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Causton : E ;1872< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&

Chappel #!, Cobb CM, Spencer !, Eick FD ;1882< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Chiba M )toh L and Bakumoto S ;1878< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/ 82 Chow - C , :rown B E ;185,< cited $ Clinical application of enamel adhesives by D " #etief >perative Dentistry, Supplement 4, 188( 22/28

Cobb E 1 :losser # - :owen #- and Fohnston + D ;1878< $ cited / 'erric o*alate with nitric acid as a conditioner in an adhesive bonding system Fournal of +dhesion (7 21/28 Cotting + , "err ! ;187&< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( Craig #0 ;188,< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Dluke E S and -inemuth F ;188&< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/82

11,

Donnan and :all ;1877< cited / LennedyCs !ediatric >perative Dentistry 2 th Edition Fohn Bright and Sons -td , 188%E %,/55

Duke E S , -indemuth F ;1881< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( Eick F D , Bilko # + , +nderson C " , Soreven S E ;185&< Scanning election microscopy of cut tooth surfaces and identification of debris by use of electron microprobe Fournal of Dental #esearch 28G 1,48/1,%7 Eick F D ;188(< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& Eidelman et al ;1872< cited / LennedyCs !ediatric >perative Dentistry 2th Edition Fohn Bright and Sons -td , 188%E %,/55 Eric C Sung , Eddie T Tai , Toni $ Chen ;(&&(< Effect of irrigation solutions on dentin bonding agents and restorative shear bond strength F !rosthet Dent (&&(E %(7/%,( Erickson ;1878< cited $ surface interactions of dentin adhesive materials by # Erickson >perative Dentistry, Supplement 4, 188(, 71/82 Erickson # - , 0lasspoole E + and !ashley ;1881< cited $ surface interactions of dentin adhesive materials by # - Erickson 188(, 71/82 Erickson # ;188(< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( >perative Dentistry, Supplement 4,

112

'an3uin and :rouillet ;1877< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/ 15% 'u.itani ;187%< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/15% 'usayama T , 1akamura M , Lurosaki 1 ;1858< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* Supplement 4, 188(, 1%4/15% 'usayama T , 1akamura T , Lurosaki 1 ;1858< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/ 14& 'usayama ;187&< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/15% 'usayama T ;187&< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( 0arberoglio #, :rannstrom M ;185%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 0uba C F , Cochran M + , Swart9 M - ;1882< Dentistry 18G 12%/14, The effects of varied etching time >perative Dentistry,

and etching solution viscosity on bond strength and enamel morphology >perative

0winnett + F , Matsui + , :uonocore M 0 ;18%8< cited $ Clinical application of enamel adhesives by D " #etief >perative Dentistry, Supplement 4, 188( 22/28

114

"amilton BF, Fudd 0, +nell 0S ;185,< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 "amlin ! , -ynch E , Samarawickrama ;188&< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/ (2( "amlin ! , -ynch E , Samarawickrama D ;1888< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 "anks C T , Craig # 0 , Diehl M - ;1877< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( "anning M , #einhardt L F , :ott : ;1882< Self etching primer 6s phosphoric acid an alternative concept for composite to enamel bonding >perative Dentinstry (2, 15(/17& "ensten !ettersen + ;1875< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 "osoda " and 'usayama T ;1872< cited $ )nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&

"osada " , "iraswa L and 'u.itani M ;1878< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/ 14& "osada " 'u.itani T 1egishi T and "irasawa L ;1878< / cited / Effect of a series of new cavity treatment on bond strength and wall adapt ion of adhesive composite resins Fapaness Fournal of Conservative Dentistry ,(G %4%/%%4
11%

"ume B # , Mount 0 F ;1877< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( )chi.o T, Iamashita I, Terashima T ;188,< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 )ngaki + , Chigara " , )toh ;1878< / cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/82 )nokoshi S "arnirattisai C Shimada I Tatsumi T and "osoda " ;1878< $ cited / Study on resin impregnated layer of various dentin bonding techni3ues Fournal of Fapanese Society for Dental Materials and Devices 7 Special )ssue 12 84/8% )noue T , Shimono M ;188(< / cited / The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( Fohnson D C ;188&< )nnervation of teethG developmental aspects )nG )noki # Luda T, >lgart -, eds Dynamic +spects of Dental !ulp 1,/(7 Chapman and "allG 1ew Iork Fohnson # " , Christensen 0 F , Stigers # B ;185&< / cited / !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Fohnson + D, +smussen E and :owen # - ;1878< / cited / Substitutes for 1/ phenylglycine in adhesive bonding to dentin Fournal of Dental #esearch %7 1,,5 $ 1,22 Limberly C -, :yers M # ;1877< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15

115

Linney F " , :alooch M, "aupt D - et al ;1884< Mineral distribution and dimensional changes in human dentine during deminerali9ation Fournal of Dental #esearch 52G 1158/72 Liyomura M ;1875< cited $ surface interactions of dentin adhesive materials by # Erickson >perative Dentistry, Supplement 4, 188(, 71/82 Lodaka T, 1aka.ima ', "igashi S ;1878< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Loibuchi " ;(&&1< cited bonding to dentin with a self etching primer The effect of smear layers Dental Materials 15, 1((/1(% Lramer # " , Mc-ean F B ;184(< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/15%

-egler - # , #etief D " , :radley E - ;1878< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/ 14& -settembrine - , :oylan # , Strassler " ;1885< + comparison of antimicrobial

activity of etching used for a total etch techni3ue >perative Dentistry (2G 72/77 Macko D F , #utberg M , -angeland L ;1857< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Marshall 0B, Marshall SF, Linney F", :alooch M ;1885< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15
117

Mar9ouk M + >perative Dentistry $ Modern theory and practice +cid conditioning of surface enamel 171/17, Matthews : ;188%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Meryon S D ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Miyasaka L , 1akabayashi 1 ;1888< Combination of EDT+ conditioner and phenyl !J "EM+ self etching primer for bonding to dentin Dental Materials 14, 14,/145

M.or )+, 1ordahl ) ;188%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 M.or )+ ;1874< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Mortimer ;185&< cited / LennedyCs !ediatric >perative Dentistry 2 th Edition Fohn Bright and Sons -td , 188%E %,/55

1akabayashi 1 Lo.ima L and Masuhara E ;187(< / cited / The promotion of adhesion by the infiltration of monomers into tooth substrates Fournal of :iomedical Materials #esearch 1% (%4/(5, 1akabayashi 1 ;1874< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/82 1akabayashi 1 ;1878< cited $ Surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/82
118

1akabayashi 1 ;1878< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& 1akabayashi 1 ;1881< / cited / The hybrid layer as a dentin/bonding mechanism Fournal of Esthetic Dentistry ,;,< (%/,1

1ewman "1, !oole D'0 ;1852< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 1ordenvall L F , :rannstrom M , Torstenson : ;1858< $ cited !ulpal considerations of adhesive materials by "arold # Stanley 188( 141/1%2 >rams "F, Kybert FF, !hakey !p, #achinger B+ ;185%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 >rchardson #, Collins BF1 ;1875< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 >sborn FB ;18%7< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !ashley D " ;1858< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 !ashley and Michelich ;1871< cited $ )nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&
1(&

>perative Dentistry, Supplement

4,

!ashley D " , Michelich 6 , Lehl T ;1871< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2(

!ashley ;187,< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( !ashley D " ;1872< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& !ashley D" ;1874< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !ashley and 0allowa. ;1874< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( !ashley D " ;1874< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 !ashley D " ;1874< $ cited / Dentin/predentin comple* and its permeabilityG physiologic overview Fournal of Dental #esearch %2 Special issue %1,/%(& !ashley D " , Depew D D ;187%< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 !ashley D " ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2

!ashley D " , Tao - , :oyd ;1877< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( !ashley D" ;188&< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15
1(1

!ashley D " ;1881< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& !ashley D", !ashley E- ;1881< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !ashley E - , Talman , "orner # ;1881< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( !ashley D " , Michelich 6 , Lehl ;1881< cited $ surface interactions of dentin adhesive materials by # - Erickson >perative Dentistry, Supplement 4, 188(, 71/ 82 !ashley D" ;188%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !ashley D", Carvalho #M ;1885< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !oole D'0, :rooks +B ;18%1< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 !ower D # , 'olleras T , Mersom S + ;187(< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 !owis D # , 'olleras T , Merson S + ;187(< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& !rati C , !ashley D M and Montanani 0 ;1881< cited $)nteractions of conditioners on the dentin surface by D " !ashley 1,5/14& >perative Dentistry, Supplement 4, 188(
1((

#etlief D " , :usscher " F , :aer ! de ;187%< + laboratory evaluation of three etching solutions Dental Materials (, (&(/(&% #ichard Tencate Te*tbook of >ral histology, development, structure and function 2th Edition "arcocourt +sia !TE -td #ipa ;18%%< cited / LennedyCs !ediatric >perative Dentistry 2th Edition Fohn Bright and Sons -td , 188%E %,/55 #obinson C, Beatherll F+, "allsworth +S ;1851< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 #upp ;1871< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 #use 1 D , Smith D C ;1881< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( Sauk F F , 6an Lampen ;1878< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& Schulein T M ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Shahabi S , Balsh - F ;1885< Effect of bonding agents on adhesion of composite resin following C>( laser etching of dental enamel F Clinical -aser Med Surgery 12, 1%8/15, ;+bstract !apers< Shellis #! ;1872< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15

1(,

Shellis #! ;1882< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Shellis #! ;188%< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Shintani " , Satou 1 , Satou F ;1878< cited $ Conditioning of the dentin substrate by # - :entolotti >perative Dentistry, Supplement 4, 188(, 1,1/1,7

Silverstone ;185&< cited / LennedyCs !ediatric >perative Dentistry 2 th Edition Fohn Bright and Sons -td , 188%E %,/55 Silverstone ;1852< cited / LennedyCs !ediatric >perative Dentistry 2 th Edition Fohn Bright and Sons -td , 188%E %,/55 Silverstone - M ;1852< cited $ Clinical application of enamel adhesives by D " #etief >perative Dentistry, Supplement 4, 188( 22/28

Silverstone - M , Sa*ton C + , Dolon ) - ;1854< cited $ Clinical application of enamel adhesives by D " #etief >perative Dentistry, Supplement 4, 188( 22/28

Silverstone -M ;187(< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Sowen #- Eichmiller ' C Mar.enhoff, B + and #upp 1 B ;1878< $ cited / +dhesive bonding of composites Fournal of the +merican College of Dentists 4%;(< 1&/1, Stagel ) , >stro E , Cesare S ;1875< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&

1(2

Stanley " # 0oing # E and Chauncey " " ;1854< $ cited / "uman pulp response to acid pretreatment of dentin and to composite restoration Fournal of +merican Dental +ssociation 81 715/7(4 Stanley " # , :owen # - , Cobb E 1 ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Stanley " # ;1878< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Stanley " # ;188&< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Sturdevant C M Theodore M #obertson, "erald > , "eyman The art and science of dentistry Dental addition (21/(27 Sui9aki F ;1881< cited $ Conditioning of the dentin substrate by # - :entolotti >perative Dentistry, Supplement 4, 188(, 1,1/1,7 Sundstrom :, Kelander T ;18%7< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Surmont ! Mareels S and Moors M ;1878< $ cited / + scorning electron microscopic and tansies bone strength evaluation of 0loms Dentin :ond application, as a function of dentinal pretreatment Dental Materials 4 ((2/((8 Takahashi M , Su9uki L , 1aka ;1881< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( Takahashi M , Su9uki L , "osada " ;1888< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2(
1(4

Tao and !ashley ;1878< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& Tao - , Tagami ) and !ashley D " ;1881< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14& Tatsumi L ;1878< !hysiological reminaral of artificially decalcified monkey dentin under adhesive composite resin restoration Lokubyo 0akkai Laishi 4%G 25/52 Tatsumi and >thers ;188(< #eminerali9ation of etched dentin Fournal of !rosthetic Dentistry %5G %15/%(& Tobias # S ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 Torneck CD ;1882< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 6an de 6oorde + , 0erdts 0 F , Mue*ision D ' ;1877< $ cited !ulpal considerations of adhesive materials by "arold # Stanley 188( 141/1%2 6an Meerbeek : , )nokoshi ;188(< cited $ The effects of acid etching on the pulpodentin comple* by David " !ashley >perative Dentistry 188(, 15, ((8/(2( >perative Dentistry, Supplement 4,

6imal L Sikri Te*tbook of >perative Dentistry C:S !ublishers and Distributors (&&(, 1st Edition, ,25/,5,

1(%

6o.inomic > , 1yborg " , :rannstrom M ;185,< $ cited !ulpal considerations of adhesive materials by "arold # Stanley >perative Dentistry, Supplement 4, 188( 141/1%2 6ongsavan 1 ;1882< cited $ Tooth wear and sensitivity $ clinical advances in restorative dentistry by Martin +ddy et al !ublished by Martin Dunit9 1 $ 15 Bhite F M , 0oodis " E , Cohen F ;1881< cited $ Conditioning of the dentin substrate by # - :entolotti >perative Dentistry, Supplement 4, 188(, 1,1/1,7 Bhite F M , 0oodis " E , #ose C M ;188&< cited $ Conditioning of the dentin substrate by # - :entolotti >perative Dentistry, Supplement 4, 188(, 1,1/1,7 Bhite and >thers ;188(< cited $ Effects of adhesive resins and various dental cements on the pulp by C ' Co* >perative Dentistry, Supplement 4, 188(, 1%4/15% Bilson + D , Mclean F B ;1877< cited $)nteractions of conditioners on the dentin surface by D " !ashley >perative Dentistry, Supplement 4, 188( 1,5/14&

1(5