Structural formulas of apatites: M(1)4M(2)6(XO4)6Z2 [2].
\r\n\tThis book intends to cover major mineral deficiency problems such as calcium, iron, magnesium, sodium, potassium and zinc. These minerals have very important task either on intracellular or extracellular level as well as regulatory functions in maintaining body homeostasis.
\r\n\r\n\t
\r\n\tBoth macrominerals and trace minerals (microminerals) are equally important, but trace minerals are needed in smaller amounts than major minerals. The measurements of these minerals quite differ. Mineral levels depend on their uptake, metabolism, consumption, absorption, lifestyle, medical drug therapies, physical activities etc.
\r\n\tAs a self-contained collection of scholarly papers, the book will target an audience of practicing researchers, academics, PhD students and other scientists. Since it will be published as an Open Access publication, it will allow unrestricted online access to chapters with no reading or subscription fees.
",isbn:"978-1-83881-085-6",printIsbn:"978-1-83881-081-8",pdfIsbn:"978-1-83881-086-3",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"8bc7bd085801296d26c5ea58a7154de3",bookSignature:"Dr. Gyula Mozsik and Dr. Gonzalo Díaz-Soto",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/8935.jpg",keywords:"Calcium, Iron, Magnesium, Potassium, Sodium, Zinc, Diagnostic tools, Treatments, Food Fortification, Malnutrition, Metabolic Disorders, Lifestyle",numberOfDownloads:741,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"May 26th 2020",dateEndSecondStepPublish:"June 16th 2020",dateEndThirdStepPublish:"August 15th 2020",dateEndFourthStepPublish:"November 3rd 2020",dateEndFifthStepPublish:"January 2nd 2021",remainingDaysToSecondStep:"9 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"Professor Emeritus of Medicine at Univesity of Pecs, Hungary, and recipient of Andre Roberts award from the International Union of Pharmacology in 2014. He published 360 peer-reviewed papers, 196 book chapters, 692 abstracts, 19 monographs, and edited 32 books.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"58390",title:"Dr.",name:"Gyula",middleName:null,surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik",profilePictureURL:"https://mts.intechopen.com/storage/users/58390/images/system/58390.jpg",biography:"Gyula Mózsik, MD,PhD, ScD(med) is a professor emeritus of medicine at First Department of Medicine, Univesity of Pécs, Hungary. He was head of the Department from 1993 to 2003. His specializations are medicine, gastroenterology, clinical pharmacology, clinical nutrition. His research fields are biochemical and molecular pharmacological studies in gastrointestinal tract, clinical pharmacological and clinical nutritional studies, clinical genetic studies, and innovative pharmacological and nutritional (dietetical) research in new drug production and food production. He published around 360 peer-reviewed papers, 196 book chapters, 692 abstracts, 19 monographs, 32 edited books. He organized 38 national and international (in Croatia ,France, Romania, Italy, U.S.A., Japan) congresses /Symposia. He received the Andre Robert’s award from the International Union of Pharmacology, Gastrointestinal Section (2014). Fourteen of his students were appointed as full professors in Cuba, Egypt and Hungary.",institutionString:"University of Pécs",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"22",totalChapterViews:"0",totalEditedBooks:"9",institution:{name:"University of Pecs",institutionURL:null,country:{name:"Hungary"}}}],coeditorOne:{id:"92633",title:"Dr.",name:"Gonzalo",middleName:null,surname:"Díaz-Soto",slug:"gonzalo-diaz-soto",fullName:"Gonzalo Díaz-Soto",profilePictureURL:"https://mts.intechopen.com/storage/users/92633/images/3485_n.jpg",biography:"Dr. Gonzalo Díaz-Soto is Associate Professor of Endocrinology and Nutrition in Medical School of Valladolid University and researcher at the Endocrinology and Nutrition Institute (IEN) at the same University. He received his MD and Master in Bioscience in experimental Endocrinology and Calcium Sensing Receptor from the Medical School of Valladolid. He finished his specialisation on Endocrinology and Nutrition Hospital Clinic of Barcelona. He currently works at the Clinical University Hospital of Valladolid in the Endocrinology, Diabetes and Nutrition Department.",institutionString:"University of Valladolid",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"1",totalChapterViews:"0",totalEditedBooks:"2",institution:{name:"Hospital Clínico Universitario de Valladolid",institutionURL:null,country:{name:"Spain"}}},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"6",title:"Biochemistry, Genetics and Molecular Biology",slug:"biochemistry-genetics-and-molecular-biology"}],chapters:[{id:"72450",title:"Parathyroid Glands and Hyperparathyroidism: A General Overview",slug:"parathyroid-glands-and-hyperparathyroidism-a-general-overview",totalDownloads:109,totalCrossrefCites:0,authors:[null]},{id:"73735",title:"Mineral Deficiencies a Root Cause for Reduced Longevity in Mammals",slug:"mineral-deficiencies-a-root-cause-for-reduced-longevity-in-mammals",totalDownloads:86,totalCrossrefCites:0,authors:[null]},{id:"73026",title:"Calcium and Metabolic Bone Disorders",slug:"calcium-and-metabolic-bone-disorders",totalDownloads:115,totalCrossrefCites:0,authors:[null]},{id:"72852",title:"Severe Hypocalcemia after Total Parathyroidectomy Plus Autotransplantation for Secondary Hyperthyroidism-Risk Factors and a Clinical Algorithm",slug:"severe-hypocalcemia-after-total-parathyroidectomy-plus-autotransplantation-for-secondary-hyperthyroi",totalDownloads:83,totalCrossrefCites:0,authors:[null]},{id:"72573",title:"Familial Syndromes of Primary Hyperparathyroidism",slug:"familial-syndromes-of-primary-hyperparathyroidism",totalDownloads:85,totalCrossrefCites:0,authors:[null]},{id:"73976",title:"Nutrigenomics: An Interface of Gene-Diet-Disease Interaction",slug:"nutrigenomics-an-interface-of-gene-diet-disease-interaction",totalDownloads:222,totalCrossrefCites:0,authors:[null]},{id:"74772",title:"Organoleptic, Sensory and Biochemical Traits of Arabica Coffee and their Arabusta Hybrids",slug:"organoleptic-sensory-and-biochemical-traits-of-arabica-coffee-and-their-arabusta-hybrids",totalDownloads:42,totalCrossrefCites:0,authors:[null]}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"184402",firstName:"Romina",lastName:"Rovan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/184402/images/4747_n.jpg",email:"romina.r@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"3317",title:"Current Topics in Gastritis",subtitle:"2012",isOpenForSubmission:!1,hash:"f771281e35f030a6438b269e736f910d",slug:"current-topics-in-gastritis-2012",bookSignature:"Gyula Mozsik",coverURL:"https://cdn.intechopen.com/books/images_new/3317.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3860",title:"Capsaicin - Sensitive Neural Afferentation and the Gastrointestinal Tract",subtitle:"from Bench to Bedside",isOpenForSubmission:!1,hash:"62e71e4f81c52b92224c231016a34231",slug:"capsaicin-sensitive-neural-afferentation-and-the-gastrointestinal-tract-from-bench-to-bedside",bookSignature:"Gyula Mozsik, Omar M. 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Abdel- Salam and Koji Takeuchi",coverURL:"https://cdn.intechopen.com/books/images_new/3860.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"5881",title:"Gastric Cancer",subtitle:null,isOpenForSubmission:!1,hash:"228701f521d44d2fff6d81063740d974",slug:"gastric-cancer",bookSignature:"Gyula Mózsik and Oszkár Karádi",coverURL:"https://cdn.intechopen.com/books/images_new/5881.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"6810",title:"Capsaicin and its Human Therapeutic Development",subtitle:null,isOpenForSubmission:!1,hash:"9b0d5832824ac89f96d0557555448206",slug:"capsaicin-and-its-human-therapeutic-development",bookSignature:"Gyula Mozsik",coverURL:"https://cdn.intechopen.com/books/images_new/6810.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"7103",title:"Constipation",subtitle:null,isOpenForSubmission:!1,hash:"0f5c714417d2c8a2e536ff6f78302cea",slug:"constipation",bookSignature:"Gyula Mózsik",coverURL:"https://cdn.intechopen.com/books/images_new/7103.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4817",title:"Membrane-bound Atp-dependent Energy Systems and the Gastrointestinal Mucosal Damage and Protection",subtitle:null,isOpenForSubmission:!1,hash:"33b0ab37b6c96db36130daafb1cd9701",slug:"membrane-bound-atp-dependent-energy-systems-and-the-gastrointestinal-mucosal-damage-and-protection",bookSignature:"Gyula Mozsik and Imre Szabo",coverURL:"https://cdn.intechopen.com/books/images_new/4817.jpg",editedByType:"Authored by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"3",chapterContentType:"chapter",authoredCaption:"Authored by"}},{type:"book",id:"7943",title:"Nutrition in Health and Disease",subtitle:"Our Challenges Now and Forthcoming Time",isOpenForSubmission:!1,hash:"bf9135b4940c5e9bf0f7de103e543946",slug:"nutrition-in-health-and-disease-our-challenges-now-and-forthcoming-time",bookSignature:"Gyula Mózsik and Mária Figler",coverURL:"https://cdn.intechopen.com/books/images_new/7943.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"6924",title:"Adenosine Triphosphate in Health and Disease",subtitle:null,isOpenForSubmission:!1,hash:"04106c232a3c68fec07ba7cf00d2522d",slug:"adenosine-triphosphate-in-health-and-disease",bookSignature:"Gyula Mozsik",coverURL:"https://cdn.intechopen.com/books/images_new/6924.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"5162",title:"The Gut Microbiome",subtitle:"Implications for Human Disease",isOpenForSubmission:!1,hash:"f21c4722be61a42e7e6ed30cb898b9ad",slug:"the-gut-microbiome-implications-for-human-disease",bookSignature:"Gyula Mozsik",coverURL:"https://cdn.intechopen.com/books/images_new/5162.jpg",editedByType:"Edited by",editors:[{id:"58390",title:"Dr.",name:"Gyula",surname:"Mozsik",slug:"gyula-mozsik",fullName:"Gyula Mozsik"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"6694",title:"New Trends in Ion Exchange Studies",subtitle:null,isOpenForSubmission:!1,hash:"3de8c8b090fd8faa7c11ec5b387c486a",slug:"new-trends-in-ion-exchange-studies",bookSignature:"Selcan Karakuş",coverURL:"https://cdn.intechopen.com/books/images_new/6694.jpg",editedByType:"Edited by",editors:[{id:"206110",title:"Dr.",name:"Selcan",surname:"Karakuş",slug:"selcan-karakus",fullName:"Selcan Karakuş"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"49963",title:"Substituents and Dopants in the Structure of Apatite",doi:"10.5772/62213",slug:"substituents-and-dopants-in-the-structure-of-apatite",body:'\nAs was already said in Chapter 1, the generic formula of apatite (M10(XO4)6Z2) enables partial or complete substitution for cationic as well as anionic sites [1],[2]:
Cation substitution, where M = Ca2+, Pb2+, Sr2+, Mg2+, Fe2+, Mn2+, Cd2+, Ba2+, Co2+, Ni2+, Cu2+, Zn2+, Sn2+, Eu2+, Na+, K+, Li+, Rb+, NH4+, La3+, Ce3+, Sm3+, Eu3+, Y3+, Cr3+, Th4+, U4+, U6+ and □.
Substitution for phosphorus by one or two cations, where X = PO43−, AsO43−, SiO43−, VO43−, CrO43−, CrO42−, MnO43−, SO42−, SeO42−, BeF42−, GeO44−, ReO53−, SbO3F4−, SiO3N5−, BO45−, BO33− and CO32−.
Z-site substation, where Z = F−, OH−, Cl−, O2−, O3−, NCO−, BO2−, Br−, I−, NO2−, CO32−, O22−, O2−, S2−, NCN2−, NO22− and □.
where □ represents the vacancy cluster [1].
\nBesides the monoionic substitution, the co-substitution and mutual combinations of substitutions in anionic and cationic sites (multi-ionic substitution) were also often reported [3],[4],[5],[6]. Mutual substitutions of trace elements into apatite structure brought new physicochemical, mechanical and biological properties in comparison with pure apatite or monoionic substituted apatite materials, e.g. hydroxylapatite [3].
\nSome substitutions can proceed only at the synthesis stage, while a limited ion exchange between solid apatite and surrounding solution can also occur. Due to their high chemical diversity and ion-exchange capabilities, apatites are considered as materials for toxic waste storage and for wastewater purification. The ion exchange in apatitic structures in human organism also presents an interest for medicine [7].
\nRecent studies have shown that a number of alkaline-earth-rare-earth silicates and germanates also have the apatite structure, and these have the cell sizes which span the division between the “apatites” and the “pyromorphites”. Some, particularly barium and lanthanum apatites, have the lattice parameters comparable with the members of the pyromorphite group. Thus, Ba2La8(SiO4)6O2 has the cell parameters a = 9.76 Å and c = 7.30 Å and Pb10(PO4)6F2 shows a = 9.76 and c = 7.29 Å, while Ba3La7(GeO4)6O1.5 has a = 9.99 Å and c = 7.39 Å and Pb10(AsO4)6F2 has a = 10.07 Å and c = 7.42 Å. During synthetic studies, however, it became apparent that the prediction of the composition of compounds with apatite-type structures could not be made solely on the basis of satisfying the valence considerations, since the occurrence of the apatite-type structure also appears to be determined by the ratio of the mean size of “A” ions (i.e. Ca ions in fluorapatite) to the mean size of “X” ions in XO4 [8],[9].
\nThe ionic radius of elements that can be accommodated instead of M in the lattice of apatite (M5(XO4)3Zq).
The structure of hydroxyapatite allows large variations from its theoretical composition as well as the formation of nonstoichiometric forms and ionic substitutions. More than half of naturally occurring elements are known to be accommodated in the apatite lattice to significant extent. Ca2+ cation can be substituted by Na+, K+, Mg2+, Sr2+, Pb2+, Mn2+ (Fig. 1(a)) or rare-earth elements[1] - (REE, Fig. 1(b)) and PO43− anions by AsO43−, SO42− or CO32− without destroying the apatite structure. The changes in lattice parameters must be indicative of the type of substitution occurring. For example, Cl− interchange for OH− ions causes a change to lattice parameters from a = 9.4214 Å and c = 6.8814 Å to 6.628 Å and 6.764 Å, respectively. Another example is the Sr2+ substitution for Ca2+, which causes lengthening of a- and c-axes from 9.418 Å and 6.884 Å to 9.76 Å and 7.27 Å, respectively [8],[12],[13],[14],[15].
\nThe substitutions at Z site play a very important role in the crystallography of specific species. The Z site lies in the channel formed by the X sites in fluorapatite and is of just the right size to fit between X atoms, and it lies on (001) mirror planes to yield the space group P63/
Some of the various families of substitutions that were experimentally established in apatites are summarized in Table 1. In general, the ions that substitute for Ca in the A position have the valences from 1 to 3 and the coordination numbers of VII at Ca(2) (6h) site and IX at Ca(1) (4f) site. Table 2 introduces the cation radii of possible apatite substituents at M-site [2].
\nM10 | \nX6 | \nO24 | \nZ2 | \nDesignation | \n
---|---|---|---|---|
M(1)4M(2)6 | \n\n | O12O6O6 | \n\n | \n |
Ca10 | \nP6 | \nO24 | \n(OH)2 | \nHAP | \n
C4Ln6 | \nSi6 | \n|||
Sr10 | \nS3Si3 | \nF2 | \nFAP | \n|
Ca2Ln8 | \nSi6 | \nO2 | \nOxyapatite | \n|
SrCa9 | \nP6 | \n□ | \nZ-site vacancies | \n|
Nd4Ca6 | \nGe6 | \n□2 | \n||
Sr10 | \nP4Si2 | \n□2 | \n||
Na2Ca8 | \nP6 | \n□2 | \n||
□2La2Ca4La2 | \n□2 | \nM-, Z-site vacancy | \n||
□2La2La2 | \nGe6 | \n\n | (OH)2 | \nM-site vacancies (?) | \n
Structural formulas of apatites: M(1)4M(2)6(XO4)6Z2 [2].
Substituents | \nCoordination number | \n|||||
---|---|---|---|---|---|---|
Arens | \nShannon and Prewitt | \n|||||
\n | \n | VI | \nVI | \nVII | \nVIII | \nIX | \n
M2+\n | \nBa | \n1.34 | \n1.36 | \n1.39 | \n— | \n1.47 | \n
Pb | \n1.20 | \n1.18 | \n— | \n1.29 | \n1.33 | \n|
Eu | \n— | \n1.17 | \n— | \n1.25 | \n— | \n|
Sn | \n0.93 | \n— | \n— | \n1.22 | \n— | \n|
Sr | \n1.12 | \n1.16 | \n1.21 | \n1.25 | \n— | \n|
Ca | \n0.99 | \n1.00 | \n1.07 | \n1.12 | \n1.18 | \n|
Cd | \n0.97 | \n0.95 | \n1.00 | \n1.07 | \n— | \n|
Mn | \n— | \n0.83 | \n— | \n0.93 | \n— | \n|
Zn | \n0.74 | \n0.745 | \n— | \n— | \n0.90 (E) | \n|
Co | \n0.72 | \n0.735 | \n— | \n— | \n— | \n|
Cu | \n0.72 | \n0.73 | \n— | \n— | \n— | \n|
Mg | \n0.66 | \n0.72 | \n— | \n0.89 | \n— | \n|
Ni | \n0.69 | \n0.69 | \n— | \n— | \n— | \n|
M+\n | \nK | \n1.33 | \n1.38 | \n1.46 (?) | \n1.51 (?) | \n1.55 (?, E) | \n
\n | Na | \n0.97 | \n1.02 | \n1.13 (?) | \n1.16 | \n1.32 (?, E) | \n
Cation radii of possible apatite substituents at M10-site of M10(XO4)6Z2 unit [2].
(E) and (?) denote interpolated and doubtful values, respectively.
An example of charge compensating substitution for phosphorus by two cations is the substitution during the synthesis of apatite species of the composition of Ca10(SiO4)3(SO4)3F2 (CSSF, fluorellestadite [16]) [2],[17],[18]:
\nThese synthetic phases have mineral equivalents in the minerals from the ellestadite group, which are listed in Table 3. Since the mineral with ideal end-member formula Ca5(SiO4)1.5(SO4)1.5Cl is assumed not to exist, the name ellestadite-(Cl) is discredited [19].
\nDescriptor | \nBrief description | \n
---|---|
a [Å] | \nLattice constant of hexagonal unit cell | \n
b [Å] | \n|
c:a | \nVariable axial ratio | \n
rMI [Å] | \nShannon’s ionic radii of M(I)-site ion (nine-coordination) | \n
rX [Å] | \nShannon’s ionic radii of X-site ion | \n
rMII [Å] | \nShannon’s ionic radii of M(II)-site ion (seven-coordination for X = F−, eight-coordination for X = Cl− and Br−) | \n
RZ [Å] | \nShannon’s ionic radii of Z-site ion | \n
Av CR [Å] | \nAverage crystal radius = [(rM(I)x4) + (rM(II)x6) + (rXx6) + (rOx24) + (rZx2))]/42 | \n
MEN - OEN | \nElectronegativity difference between M and O atom | \n
XEN - OEN | \nElectronegativity difference between X and O atom | \n
MEN - ZEN | \nElectronegativity difference between M atom at M(II) site and Z atom | \n
MEN - XEN | \nElectronegativity difference between M atom at M(I) site and X atom | \n
M(I) – O(1) [Å] | \nDistance between M(I) atom and O(1) atom | \n
M(I) – O(1)M(I)z = 0 [Å] | \nDistance between M(I) atom and O(1) atom with the constraint z = 0 at M(I) | \n
ΔM(I)−O [Å] | \nDifference in the lengths M(I) – O(1) and M(I) – O(2). | \n
\n\n | \nDifference in the lengths M(I) – O(1) and M(I) – O(2) with the constraint z = 0 at M(I) | \n
ΨM(I)−O [°] | \nAngle that M(I)-O(1) bond makes with respect to c | \n
\n\n | \nAngle that M(I)-O(1) bond makes with respect to c with the constraint z = 0 at M(I) | \n
δM(I) [°] | \nCounter-rotation angle of M(I)O6 structural unit | \n
ϕ M(I) [°] | \nMetaprism twist angle (π/3 – 2δM(I)) | \n
αM(I) [°] | \nOrientation of M(I)6 unit with respect to a | \n
<X-O> [Å] | \nAverage X-O bond length | \n
<τO−X−O> [°] | \nAverage O-X-O bond-bending angle | \n
ρM(II) [Å] | \nM(II)-M(II) triangular side length | \n
M(II) – Z [Å] | \nOrientation of M(II)-M(II)-M(II) triangles with respect to a | \n
M(II) – O(3) [Å] | \nDistance between M(II) and O3 atoms | \n
φO(3)−M(II)−O(3) [°] | \nO(3) – M(II) – O(3) angle | \n
Etotal [eV] | \nTotal energy calculated from ab initio calculations | \n
The list of 29 discrete descriptors of electronic and crystal structure parameters [23].
The fluorellestadite apatite and its solid solutions are minor components of many fluorine-mineralized clinkers. It is stable to liquidus temperature of 1240°C at which it incongruently melts to dicalcium silicate (2CaO·SiO2) and liquid [16]. The solid-state synthesis and the luminescence properties of europium-doped fluorellestadite (CSSF:Eu2+) cyan-emitting phosphor were described by
The general composition of silico-sulfate apatites, i.e. ellestadites, is Ca10(SiO4)3−x/2(PO4)x(SO4)3−x/2(F,Cl,OH)2 and their structures conform to P63/
The syntheses of Sr and Pb analogues of CSSF are also reported [18]. Strontium silico-sulfate apatite is not stable and decomposes to the mixture of strontium silicate and sulfate when heated to 1130°C for 30 min. Since high temperatures must be avoided, several attempts to prepare cadmium and barium silico-sulfate apatites were unsuccessful and the silicocarnotite-like phase was obtained from a mixture of the composition of Ca10(GeO4)3(SO4)8F2 rather than apatite [17].
\nSince there is a huge potential for the substitution in apatite structure (M(1)4M(2)6(XO4)6Z2 and for the formation of solid solution as well, the classification method enables to identify the key crystallographic parameters which can serve as strong classifiers of crystal chemistries. The structure maps for apatite compounds via data mining were reported by
Basically, the structure map approach involves the visualization of the data of known compounds with known crystal structures in a two-dimensional space using two scalar descriptors (normally heuristically chosen), which are associated with physical/chemical properties, crystal chemistry or electronic structure. The objective is to map out the relative geometric position of each structure type from which one tries to discern qualitatively if there are strong associations of certain structure types to certain bivariate combinations of parameters [23].
\nBond-distortion angle applied for the construction of structure map [23].
A new structure map, defined using the two distortion angles (Fig. 3) [23]:
1.The αMII (rotation angle of MII-MII-MII triangular units);
The
That enables to classify the apatite crystal chemistries based on the site occupancy at M, X and Z sites and this classification is accomplished using the K-means clustering analysis (Fig. 3).
\nStructure map for the classification of apatite chemistries based on the site occupancy (Table 4) at M, X and Z sites [23].
For example, clusters 1 and 2 (k = 1 and k = 2) correspond to F-apatites (fluorapatites). They are well localized in the structure map and are characterized by relatively low αMII and \n
Cluster | \nSite occupancy | \n||
---|---|---|---|
k = 1 and k = 2 | \nSite | \nM | \nBa, Pb, Sr, Ca | \n
X | \nP, V, Mn | \n||
Z | \nF | \n||
k = 3 | \nSite | \nM | \nBa | \n
X | \nP | \n||
Z | \nCl, Br | \n||
k = 4 | \nSite | \nM | \nSr, Hg | \n
X | \nP | \n||
Z | \nCl, Br | \n||
k = 5 | \nSite | \nM | \nCa, Cd, Pb | \n
X | \nV, Cr, As | \n||
Z | \nCl | \n||
k = 6 | \nSite | \nM | \nCa, Pb | \n
X | \nP | \n||
Z | \nCl, Br | \n||
k = 7 | \nSite | \nM | \nZn | \n
X | \nP | \n||
Z | \nZ | \nZ | \nF, Cl | \n
Even though Ca2+ and Hg2+ cations have roughly the same ionic size (1.18 and 1.23 Å at M(I) site), their electronegativity data indicates that Hg atoms (electronegativity value of 2 in Pauling scale) are relatively highly covalent compared to Ca atoms (electronegativity value of 1 in Pauling scale). In the structure map, this covalent character is predicted to be manifested in the bond distortion angle \n
Sr2+ ion, which is larger than Ca2+, is ordered almost completely into the smaller Ca(2) site in the apatite structure (Fig. 4). The bond valence sums of Sr ions at two sites demonstrate that Sr is severely overbonded at apatite Ca site but less at Ca(2) site. Complete ordering of Sr into Ca(2) sites has important implications for the diffusion of that element in the apatite structure. It is the subject of several recent studies. The diffusion of Sr in (001) was shown to be as rapid or even more rapid than the diffusion parallel to [001]. As there are neither sites available for Sr, which are linked in (001), nor any interstitial sites, which can contain Sr2+ ion, the diffusion mechanism involving the vacancies or defects or both is indicated [24].
\n\nA series of Sr-substituted hydroxyapatites, (SrxCa1−x)5(PO4)3OH, where x = 0.00, 0.25, 0.50, 0.75 and 1.00, was investigated by
The structure of natural Sr-bearing apatite refined by Hughes et al [24] and viewed along the c-axis.
Strontium is often substituted for calcium in order to confer the radio-opacity in glasses used for dental cements, biocomposites and bioglass-ceramics. It can be concluded that strontium substitutes for calcium with little change in the glass structure as a result of their similar charge to size ratio. Glasses with low content of strontium nucleate in the bulk to form calcium apatite phase. Glasses with medium strontium content nucleate to mixed calcium-strontium apatite at the surface and glass fully substituted by strontium to strontium fluorapatite [26].
\nMagnesium-substituted hydroxyapatite (MgHAP) powders with different crystallinity levels, prepared at room temperature via a heterogeneous reaction between Mg(OH)2/Ca(OH)2 powders and (NH4)2HPO4 solution using the mechanochemical- hydrothermal route, were reported by
Two effects of different magnesium sources (magnesium nitrate and magnesium stearate) on the synthesis of Mg-substituted hydroxyapatite (Mg-n-HAP) nanoparticles by the co-precipitation method were investigated by
Copper-substituted hydroxyapatite (Ca10−xCux(PO4)6(OH)2 (where x = 0.05 – 2.0) and fluorapatite Ca10−xCux(PO4)6F2 (x = 0.05 – 2.0) were synthesized by
According to
In this process, Ni2+ ions are first adsorbed onto the surface of hydroxyapatite (surface complexation, Section 6.5.2) and then the substitution of Ca2+ for Ni2+ ions takes place.
\nZinc is a common bioelement. The zinc content in human bones ranges from 0.0126% to 0.0217% by weight [7]. Zinc as a cationic substituent in hydroxyapatite provides the option to counteract the effects of osteoporosis [31]. The incorporation of zinc into the HAP structure (Zn-HAP) was abundantly studied, owing to the key effect of Zn2+ cations in several metabolic processes that makes zinc eligible for use in many biomedical applications and to its possible antimicrobial activity [3].
\nThe results of structure analysis indicated that Zn ions substituted partially for Ca ions in the apatite structure and the upper limit of Zn substitution for Ca in HA was about 20 mol.%. In general, the HAP lattice parameters, a and c, decreased with Zn addition [32].
\nZn-substituted apatite was synthesized by the precipitation method as follows [33]:
where 0 ≤ x ≤ 1. The pH of the solution was adjusted to 8 by aqueous solution of NH3, and the reaction mixture was kept at 90°C for 5 h with stirring. The resulting suspension was then subjected to suction filtration, and the powdery product was dried at 100°C for 10 h. It is known that the usage of chloride or nitrate of calcium as a starting reagent may cause the incorporation of Cl− or NO3− into the structure of apatite. This can be avoided by the utilization of acetate salts, because acetate ions are not incorporated into the apatite, i.e. they would not affect the apatite structure.
\nThe synthesis and the characterization of iron-substituted hydroxyapatite via a simple ion-exchange procedure were described by
The synthesis and the characterization of cobalt-substituted hydroxyapatite (Co-HAP) powders via the precipitation method were described by
Single crystals of chlorapatite [Ca5(PO4)3Cl] with the substitution of approximately 20% of Ca2+ by Co2+ (space group P63/
Naturally occurring manganese-substituted apatite is known as manganese-bearing apatite (Mn,Ca5(PO4)3F, Section 1.1). According to the findings of
The structure of natural Mn-bearing apatite refined by Hughes et al [24] and viewed along the c-axis.
It is interesting to note that apatite acts effectively as a geochemical sieve that traps Mn2+ and excludes Fe2+ elements, which are virtually inseparable in most geochemical systems. The bond valence sums for Fe2+ at apatite Ca sites yield 1.26 and 1.19 valence units for Ca(1) and Ca(2) sites, respectively; large discrepancy from the formal valence prohibits extensive substitution of Fe2+ in the apatite structure (Fig. 5) [24].
\nThe crystal structure of pale blue transparent Mn-rich fluorapatite (9.79 wt.% of MnO) with optimized formula (Ca8.56M2+1.41Fe2+0.01)P6O24F2 was resolved by
Crystals of La-, Gd- and Dy-bearing fluorapatite [La-FAP, Gd-FAP, Dy-FAP, Ca10−x−2y NayREEx+y(P1−ySixO4)Z2, where x = 0.24 – 0.29 and y = 0.32 – 0.36] were synthesized by hydrothermal route by
The structure of some REE-bearing apatites [37],[38] is shown in Fig. 6.
\nRare-earth-element ordering and structural variations in natural rare-earth-bearing fluorapatites (a), LaFAP (b), NdFAP (c), GdFAP (d) and DyFAP (e) [37],[38].
The partitioning of REE between two Ca positions in apatite contradicts usual first-order dependence on spatial accommodation, with LREE[1] - [39],[40],[41],[42],[43], in particular, favoring the smaller Ca(2) position. This behavior was variously ascribed to the control via [37]:
Substitution mechanism;
Electronegativity difference;
Bond valence.
The preference of individual REE among multiple Ca positions in minerals (the site occupancy of individual REE) was not extensively studied because of the inability of conventional diffraction methods to distinguish among individual elements at multiply-occupied sites. The site preference for individual LREE from theoretical bond-valence sums was estimated by
The isomorphic substitutions of neodymium for strontium in the structure of synthetic Sr5(VO4)3OH apatite structure type (P63/
where x = 0, 0.02, 0.08, 0.10, 0.12, 0.14, 0.16, 0.18 and 0.20. The substitution scheme can be expressed as:
The procedure includes three stages:
Preparation of solution;
Thermolysis;
Treatment of the dry residue.
The solutions for the thermolysis were prepared by dissolving Sr(NO3)2 in water; Nd2O3 was dissolved in water with nitric acid added; NH4VO3 was dissolved in water with hydrogen peroxide added. Dry residues after concentrating the solutions were pestled in an agate mortar and calcined with the temperature steadily raised from 600 to 800°C and intermittent grindings [44].
\nThorium and uranium (actinides [45],[46][1] -)-bearing apatites were synthesized by
The structure of UFAP (a), ThFAP (b), UClAP (c), ThClAP (d), ThSrFAP (e) and ThSrClAP (f) [47] viewed along the c-axis.
The structure refinements of U-doped chlorapatites show that U is essentially distributed equally between the two Ca sites with UCa(2)/UCa(1) values, which range from 0.89 to 1.17. The results of Th-doped chlorapatites show that Th substitutes into both Ca(1) and Ca(2) sites with ThCa(2)/ThCa(1) values, which range from 0.61 to 0.67. In Th-doped strontium apatites with F and Cl end-members, Th is incorporated into both Ca(1) and Ca(2) sites. The range of ThCa(2)/ThCa(1) values is 0.56 to 1.00 for the F end-member and 0.39 to 0.94 for the Cl end-member. U-doped samples indicate that U in fluorapatite is tetravalent, whereas, in chlorapatite, it is heterovalent but dominantly hexavalent [47].
\nBased on the chemical analyses of U-, Th-doped fluor-, chlor- and strontiumapatite specimens in this study, local charge compensation may be maintained by the following coupled substitutions (M represents U or Th and [] represents the vacancy) [47]:
The incorporation of U and Th into fluorapatite results in a decrease of the size of both Ca polyhedra, but the incorporation of U and Th into chlorapatite gives rise to an increase in the volume of both Ca polyhedra. The decrease of both Ca polyhedral volumes in fluorapatite caused by the substitution of U and Th can be explained by the decrease of ionic radius from Ca to U and Th. However, the increase in the volume of both Ca polyhedra in chlorapatite is hard to understand. Because of the effect on Ca(2) polyhedron caused by the replacement of F− by Cl−, it can be explained by the structural distortion of Ca(2) polyhedron [47].
\nUranium-doped oxy-silicophosphates (britholites) of the composition of CaxLay(SiO4)6−u (PO4)uOt:U4+ were synthesized by
or
where An4+ substitutes for tetravalent U4+ and Th4+.
\nThe incorporation of thorium in the structure is probably possible due to small differences of ionic radius between calcium (1.06 Å), neodymium (1.05 Å) and thorium (1.00 Å). In order to ensure the quantitative incorporation of thorium, it appeared necessary to consider the coupled substitution [50].
instead of the substitution scheme:
Indeed, in the first way, homogeneous and single-phase solid solutions were prepared from Ca9Nd(PO4)5(SiO4)F2 to Ca9Th(PO4)4(SiO4)2F2 leading to full neodymium substitution. Associated small increase of the unit cell parameters results from the simultaneous replacement of phosphate groups by bigger silicate. It was accompanied by a significant change in the grain morphology. These results contrast with those obtained when the coupled substitution according to Eq. 19 was performed, which confirmed the limitation of about 10 wt.% in the Th substitution [50]. Good resistance of the materials to influence of aqueous solutions enables their utilization for the immobilization of tetravalent actinides in phosphate ceramics [49].
\nThe favorable biocompatibility of hydroxyapatite (HA) makes it a popular bone graft material as well as a coating layer on metallic implant. One common and accepted strategy to prevent the implant-related infections is to create antibacterial properties for the implant. Silver ions can be either incorporated into the apatite during the co-precipitation process (AgHAP-CP) or subjected to the ion exchange with calcium ions in apatite (AgHAP-IE). The incorporation of silver ions into apatite is based on the equation [51]:
where y is the molar amount of silver to be incorporated. However, the distribution of silver ions in AgHAP-CP and AgHAP-IE was different, thus affecting the antibacterial action.
\nThe absorption of cadmium cations in apatites is relevant both from the medical standpoint of cadmium uptake by human bones, as well as since cadmium migration in nature involves the absorption and desorption equilibria with natural minerals, including apatites. Cadmium has a slight preference for Ca(I) site in fluorapatite and for Ca(II) site in hydroxyapatite [7],[52]. The interactions between these two ions (Cd and Ca) during absorption and ionic change processes in apatites present therefore considerable practical and theoretical interest. Cadmium is also a frequent heavy toxic pollutant element in water [7].
\nCalculated energy differences (E) between these sites are of 12 and 8 kJ·mol−1 for fluorapatite and hydroxylapatite, respectively. The preference is not strong, and however, a part of the sites of the other type is also occupied by cadmium ions. The relative site occupation can be expressed by the equation [7]:
where E = E(Cd2+ or Zn2+ on Ca(1)) – E(Cd2+ or Zn2+ on Ca(2)). At T = 298 K, P = 85 and 17 Cd2+ in fluorapatite and hydroxylapatite, respectively. From the value of P and from the fact that the sum of the two probabilities is 1, one can calculate that the probability of the lower-energy site occupancy is of 99% and 94%, respectively.
\n\n
Pentavalent arsenic, vanadium and chromium substitution can completely replace phosphorus in calcium, strontium and barium fluor- and chlorapatites. Calcium fluor-vanadate, -arsenate and -chromate structures were distorted compared to normal hexagonal apatite. Manganese completely replaced phosphorus only in barium apatites, while chromium and manganese could not be incorporated into lead apatites. Excluding these exceptions, continuous solid solutions were formed between the phosphate and/or vanadate and the chromate or manganese analogues for given divalent and halide ions [54]. The substitution of CO32− ions at X- (carbonate-apatite of A-type) and Z-site (carbonate-apatite of B-type) was already described in Section 4.6.
\nThe arsenate (As5+) substitution in the hydroxylapatite structure was examined by
Complete PO43− ↔ AsO43− substitution was also recognized in experimental studies of apatite analogues, such as in the system Sr5(PO4)3OH-Sr5(AsO4)3OH [58]. The Rietveld refinement of Sr5(AsO4)3Cl (pentastrontium tris[arsenate(V)] chloride, 890.31 g·mol−1) from high-resolution synchrotron data was performed by
The structure of Sr5(AsO4)3Cl apatite (perspective view along the c-axis).
The synthesis of synthetic alkaline-earth vanadate hydroxylapatites from hydroxide fluxes was performed by
The structure of Sr5(VO4)3OH (a) and Ba5(VO4)3OH (b) apatite viewed along the c-axis.
The compounds (solid solution) of the composition of Pb5(PxV1−xO4)3Cl (0 ≤ x ≤ 1), which are synthetic analogues of minerals pyromorphite, vanadinite and endlichite, were synthesized for the first time by
Fragment of Pb5(VO4)3Cl crystal structure [61].
The variations of unit cell parameters as a function of composition respect Vegard’s law. These compounds are structurally built of discrete phosphate or vanadate tetrahedra linked to one another by lead polyhedra, which form joint layers (Fig. 10). Apatite-type structures offer typically two crystallographic positions for cations differing in the coordination number and local symmetry. Lead atoms occupying the first positions form polyhedra shaped as three-capped trigonal prisms of PbO9 having the symmetry C3, the columns of which run along the threefold axis. Distorted two-capped trigonal prisms of PbO6Cl2 residing in the second positions have local symmetry С1.
\nThe syntheses of chromium (Cr(V) [62]) analogues of apatite were described in literature including the following compounds [63],[64],[65],[66],[67],[67],[69],[70],[71],[72]:
Ca5(CrO4)3OH, which is isomorphous to hydroxyapatite (Section 1.5.2): space group P63/
Sr5(CrO4)3OH with predicted lattice constants a = 9.9561 Å and c = 7.488 Å.
Ba5(CrO4)3OH.
Ca5(CrO4)3F with predicted lattice constants a = 9.733 Å and c = 7.0065 Å
Ca5(CrO4)3Cl with predicted lattice constants a = 10.1288 Å and c = 6.7797 Å.
Sr5(CrO4)3F with predicted lattice constants a = 9.9349 Å and c = 7.5037Å.
Sr5(CrO4)3Cl with lattice constant a = 10.125 Å and c = 7.328Å.
Sr5(CrO4)3Br with predicted lattice constants a = 10.2895 Å and c = 7.2712 Å.
These compounds are in general prepared by the ignition of mixture of alkaline-earth carbonates, hydroxides or oxides with Cr2O3 in the presence of water vapor. Ca3(CrO4)2 compound (orthochromate), which is isomorphous with Ca3(PO4)2, is formed as an intermediate by carrying out the synthesis in dry atmosphere; this compound is often identified as 9CaO·4CrO3·Cr2O3 [63],[73],[74],[75].
\nTheoretical compositions and formula weights of chromium apatite analogues are given in Table 5.
\nCompound | \nComposition [wt.%] | \nM | \n||||
---|---|---|---|---|---|---|
M | \nCr | \nO | \nZ | \nH | \n[g.mol−1] | \n|
Ca5(CrO4)3OH | \n35.44 | \n27.59 | \n36.79 | \n— | \n0.18 | \n565.39 | \n
Sr5(CrO4)3OH | \n54.55 | \n19.42 | \n25.90 | \n— | \n0.13 | \n803.09 | \n
Ba5(CrO4)3OH | \n65.29 | \n14.83 | \n19.78 | \n— | \n0.10 | \n1051.64 | \n
Ca5(CrO4)3F | \n35.32 | \n27.49 | \n33.84 | \n3.35 | \n— | \n567.38 | \n
Ca5(CrO4)3Cl | \n34.33 | \n26.72 | \n32.88 | \n6.07 | \n— | \n583.33 | \n
Sr5(CrO4)3F | \n54.42 | \n19.37 | \n23.85 | \n2.36 | \n— | \n805.08 | \n
Sr5(CrO4)3Cl | \n53.33 | \n18.99 | \n23.37 | \n4.31 | \n— | \n821.53 | \n
Sr5(CrO4)3Br | \n50.59 | \n18.01 | \n22.17 | \n9.23 | \n— | \n865.98 | \n
Theoretical compositions of chromium apatite analogues (M(CrO3)4Z).
Sr10(CrO4)6F2 possesses typical hexagonal structure of apatite with the space group P63/
Structural representation of Sr10(CrO4)6F2 apatite with SrO6 octahedra and CrO4 tetrahedra: larger and smaller spheres mark F and O atoms, respectively. The unit cell is indicated by black lines [71].
The crystal structure (Fig. 12) and the magnetic properties of strontium chromate phase (Sr5(CrO4)3(Cu0.586O)) with apatite-like structure were determined by
Crystal structure of Sr5(CrO4)3(Cu0.586O): (a) projection along the c-axis and (b) side view showing the infinite [CuO]− chains and the coordination polyhedra of Cr and Sr atoms [76].
This phase crystallizes in the space group P63/
Selenium oxyanion-substituted hydroxyapatite (SeHAP) was synthesized as a promising material for the treatment of bone cancer to reduce the probability of recurrence, because selenium plays an important role in protein functions and it has significant effect on the induction of cancer cell apoptosis [77]. Another study indicated that selenite (SeO42−) or selenite (SeO32−) oxyanions exert their cancer chemopreventive effects by direct oxidation of critical thiol-containing cellular substrates and that they are more efficacious anticarcinogenic agents than selenomethionine or selenomethylselenocysteine with a lack of oxidation capability [3],[78].
\nSelenium was incorporated into the hydroxyapatite lattice by replacing some of the phosphate groups with selenite groups. SeO42− (selenate) ion has tetrahedral structure like PO43− ion (Fig. 5 and Table 4 in Section 1.2), but it is slightly larger (2.49 Å) in diameter than phosphate ion, which is 2.38 Å in diameter. By contrast, SeO32− (selenite) ion has very similar diameter (2.39 Å), but it has a quite different flat trigonal pyramid geometry. The substitution of bivalent selenium oxyanions forms positively charged vacancy compensated by simultaneous decalcification and dehydroxylation according to the reaction [3],[79]:
The SeHAP crystal lattice parameters increased slightly as the Se concentration increased when the Se/P ratios were less than 0.5 [80]. All samples prepared via the precipitation method from aqueous solution by
Nitrogen was incorporated into hydroxyapatite by dry ammonia treatments at temperatures between 900 and 1200°C in the presence of graphite. The process of synthesis of cyanamidapatite (Ca10(PO4)6CN2, Ca10(PO4)6NCN) can be described by the following chemical equations [13]:
Ammonia reacts with graphite during the thermal treatment forming [CN2]2− ions (Eq. 24). These cyanamide ions interchange with moveable OH− ions situated on the sixfold screw axis of apatite to form cyanamidapatite (Eq. 25). A similar reaction is known for the synthesis of calcium cyamide from calcium oxide:
The treatments at temperatures above 1200°C or long-term treatments destroy the apatite lattice completely through the phosphate reduction. Cyanimide ions lose their sites in the apatite lattice and the nitrogen content decreases [13]. The synthesis of Ca10(PO4)6CN2 apatite provides the evidence that the hydroxylapatite structure is able to incorporate larger organic molecules [81].
\nDirect transformation of TCP (Ca3(PO4)2) into cyanamidapatite according to the reaction:
was also proposed by
Although “oxygenated” apatites were not much investigated compared to other substituted apatites, some past studies have, however, reported the possibility of apatitic channels to incorporate oxygenated species such as H2O2 or O2 or molecular ions including O22− (the peroxide ion) and superoxide O2−. They are single-phase nanocrystalline apatites, where part of apatitic OH− ions are replaced by oxygenated species. Typically by peroxide ions (quantified) and at least the traces of superoxide ions can be prepared by the precipitation from aqueous calcium and phosphate solutions in the presence of H2O2 under medium room temperature [83],[84].
\nThe local structure of hydroxyl-peroxy apatite was described by
According to the concentration of peroxide ions in hydroxyl-peroxy apatite and the theoretical value, the corresponding formula for the hydroxyl-peroxy apatite is proposed as follows [85]: Ca10(PO4)6(OH)1.34−2x(O2)0.33(O)x□0.33+x.
Possible configuration of hydroxyl ions, peroxide or oxide ions and vacancies in the channel along the crystallographic c-axis in hydroxyl-peroxy apatite. O, H atoms and vacancies are presented by large gray circles, small open circles and gray squares, respectively. Filled small circles represent H atoms perturbed by the incorporation of peroxide ions [85].
A scheme of possible configurations of hydroxyl ions, peroxide or oxide ions and vacancies in the channel along the crystallographic c-axis in hydroxyl-peroxy apatite is illustrated in Fig. 13. Peroxide ions incorporated into HAP are located in the channel of apatite structure through the substitution of a portion of OH− radicals, and the material is a solid solution of hydroxyl- and peroxide apatite.
\n\n
where [] was the vacancy. O2− ion was active and could react with O2 to produce O22−.
Peroxide ions associated with the vacancies were situated placed in the channel of HA lattice along the c-axis through the substitution of a portion of OH radicals. The molecular ions constituted a symmetric vibrator with a stretching vibration active in Raman spectrometry. This vibration was recorded at 750 cm−1 in the Raman spectra of O22−-containing HA samples. The final product was a solid solution of hydroxyl- and peroxide-apatite. However, the existence of peroxide ions in the HA lattice caused the contraction of the unit-cell dimensions of HA materials. In addition, a new hydrogen bond was formed between peroxide ions and adjacent OH radicals, which was determined by using molecular spectroscopy analysis. During annealing treatment in air, peroxide ions decomposed and the substituted OH radicals re-entered the HA lattice, resulting in the elimination of the structural aberrations caused by the incorporation of peroxide ions. The concentration of peroxide ions present in HA samples was measured by chemical analysis [86].
\nThe synthesis and the structure of four new chalcogenide[1] - [87] phosphate apatitic phases of the composition given by the formula:
Ca10(PO4)6S: a = 9.4619 Å, c = 9.8342 Å, c:a = 0.7223 and V = 529.88 Å3 (Fig. 14(a));
Sr10(PO4)6S: a = 9.8077 Å, c = 9.2089 Å, c:a = 0.7350 and V = 600.53 Å3 (Fig. 14 (b));
Ba10(PO4)6S: a = 10.2520 Å, c = 7.6590 Å, c:a = 0.7471 and V = 697.14 Å3 (Fig. 14(c));
Ca10(PO4)6Se: a = 9.5007 Å, c = 9.8406 Å, c:a = 0.7200 and V = 534.73 Å3 (Fig. 14 (d)).
were reported by
The structure of Ca(PO4)6S (a), Sr(PO4)6S (b), Ba(PO4)6S (c) and Ca(PO4)6Se (d) viewed along the c-axis.
These four apatites are isostructural and crystallize in the trigonal space group P3 over bar with the chalcogenide ion positioned at (001/2). Sulfoapatites show no ability to absorb H2S in the way that oxyapatite absorbs H2O at elevated temperatures. This can be attributed to the position of sulfide ion and the way it influences the crystal structure around vacant chalcogenide position at (000) [88].
\nStrontium borate-phosphate Sr10(PO4)5.5(BO4)0.5(BO2)[1] - was prepared from SrCO3, NH4H2PO4 and H3BO3 at high temperature (from 1150 to 1550°C) and was found to be free of alkali metal compounds. Sr10(PO4)5.5(BO4)0.5(BO2) phase is a derivative of the apatite crystal structure with metaborate ion at Z-site: space group P3, a = 9.7973 Å, c = 7.3056 Å, V = 607.29 Å3, Z = 1 [89],[90],[91].
\nThe strontium sites are found to be fully occupied, while [PO4]3ˉ tetrahedra are partially replaced by [BO4]5ˉ groups. The crystal structure contains Sr cations occupying the 6g (Sr(1)) and 2d (Sr(2), Sr(3)) sites, isolated tetrahedral [PO4]3ˉ/[BO4]5ˉ groups and linear [BO2]ˉ groups located in hexagonally shaped (trigonal antiprismatic) channels formed by Sr(1) atoms and running along [001] (Fig. 15). The space group of the present compound is reduced to P3, because the orientation of the [PO4]/[BO4] tetrahedra destroys the mirror plane characteristic for the apatite crystal structure (P63/
Crystal structure of Sr10(PO4)5.5(BO4)0.5(BO2): projection along [001] showing the hexagonally shaped channels formed by Sr(1) around the threefold inversion axis (Z = (P0.95B0.05) (a) and side view emphasizing the linear [BO2]− groups and the corresponding trigonal antiprisma formed by Sr(1) (b) [89].
Crystalline solid solutions[1] - [92] of apatites are frequently encountered where the possibility and type depend on the condition of formation or preparation, thermal history after formation and the end-members of the series [2]. The structure of ternary solid solution of hexagonal (P63/
The solid solution in hexagonal ternary apatite is achieved by a 0.4 Å shift along the c-axis of Cl atom relating to its position in end-member chlorapatite. This adjustment affects the Markovian sequence[1] - [94] of anions in the (0,0,z) anion columns by providing a structural environment that includes column OH species at the distance of 2.96 Å from Cl. The shift of Cl atom is accompanied by splitting of Ca(2) atoms into two distinct positions as a function of the kind of anion neighbor (F or OH vs. Cl). Additional nonequivalent Cl site, similar to that in end-member chlorapatite, is also present. Those Cl atoms with adjacent OH occupy a site different from Cl atoms adjacent to vacancies in the anion column [93].
\nReduction of symmetry in monoclinic ternary apatite results from the ordering of Cl and OH within the anion columns. The atomic positions of Cl and OH in the anion column are equivalent to those in hexagonal ternary apatite, but each is ordered into only one of the two hexagonal symmetry-equivalent sites [93].
\nThe apatite supergroup minerals of the solid solution [95]:
where x = 0 – 3 and y = 0 – 1.5 were found in altered calcareous xenoliths within the ignimbrite of the Upper Chegem caldera, Northern Caucasus, Russia. These minerals belonging to the apatite supergroup occur in all zones of skarn from the core to the contact with ignimbrite as follows: brucite-marble, spurrite (Ca5(SiO4)2CO3 [96]), humite (Mg7(SiO4)3(F,OH)2 [97]) and larnite[1] - (Ca2SiO4 [98],[99],[100],[101]) zones. They are associated with both high-temperature minerals: reinhardbraunsite (Ca5(SiO4)2(OH)2 [102]), chegemite (Ca7(SiO4)3(OH)2 [103]), wadalite (Ca6Al5Si2O16Cl3 [104]), rondorfite (Ca8Mg(SiO4)4Cl2 [105]), cuspidine (Ca4(Si2O7)F2 [106]), lakargiite (CaZrO3 [107]) and srebrodolskite (Ca2Fe3+\n2O5 [108]), corresponding to the sanidinite metamorphic facies,[1] - and secondary low-temperature minerals: calcium hydrosilicates (hillebrandite [113], awfillite [114], bultfonteinite [115]), hydrogarnets [116] and minerals of the ettringite group [117].
\nThe minerals of the apatite supergroup often form elongated cracked hexagonal or pseudo-hexagonal crystals up to 250 μm in size as well as grain aggregates. A new solid-solution series was found between ellestadite and svabite-johnbaumite (±apatite) with the ellestadite type isomorphic substitution according the following scheme [95]:
where R = As5+ and P5+. The As content in investigated minerals decreases from the contact skarn zone with the ignimbrite towards the core of altered xenoliths (from 2.11 As pfu[1] - to 0), for example [95]:
Svabite:
Ca5[(AsO4)2.01(PO4)0.33(SiO4)0.33(SO4)0.33]3[F0.58(OH)0.30Cl0.12]Ʃ1;
As-bearing fluorapatite:
Ca5[(PO4)1.56(AsO4)1.06(SiO4)0.19(SO4)0.19]3[F0.59(OH)0.35Cl0.06]Ʃ1;
As-bearing hydroxylellestadite:
Ca5[(SiO4)1.25(SO4)1.25(AsO4)0.43(PO4)0.07]3[(OH)0.70Cl0.20F0.10]Ʃ1;
Si, S-bearing hydroxylapatite:
Ca5[(PO4)0.95(SO4)0.93(SiO4)0.93(AsO4)0.19]3[(OH)0.67Cl0.18F0.15]Ʃ1;
Hydroxylellestadite:
Ca5[(SO4)1.49(SiO4)1.49(PO4)0.02]3[(OH)0.74F0.13Cl0.13]Ʃ1.
The crystals of As-bearing phases belonging to the investigated solid solution are heterogeneous and small in size. Therefore, X-ray single-crystal data were obtained for only Si, S, As-bearing hydroxylapatite (see the formula above): P63/
The hydrothermal synthesis of vanadate/phosphate hydroxyapatite solid solutions of the composition of Ca10(VO4)x(PO4)6−x(OH)2, where x = 0, 1, 2, 3, 4, 5 and 6, was firstly reported by
The crystal structure of 11 samples of synthetic Na-Ca-sulfate apatite systems of the composition of Na6.45Ca3.55(SO4)6(FxCl1−x)1.55, where x = 0 – 1, was refined by
Lead apatites form a family of isomorphous compounds, and well-known members of the group are mimetite (Pb5(AsO4)3Cl, Section 1.6.7) and pyromorphite (Pb5(PO4)3Cl, Section 1.6.4). Isostructural with vanadinite Pb5(VO4)3Cl, these three constituents form a ternary system within the apatite group of P63/
A number of compounds of the mimetite Pb5(AsO4)3Cl-pyromorphite Pb5(PO4)3Cl solid-solution series were synthesized at room temperature by
Solid solutions of Pb8M2(XO4)6 lead alkali apatites were studied by
Some other examples of apatite solid solutions are listed below [2]:
Ca2Y8(SiO4)6O2 – Ca8Y2(PO4)6O2;
Ca2La8(SiO4)6O2 – Ca8La2(PO4)6O2;
Ca2Y8(SiO4)6O2 –Y10(SiO4)4(BO4)2O2;
Mg2Y8(SiO4)6O2 – Y10(SiO4)4(BO4)2O2;
Pb4+\n3Pb2+\n5Y2(SiO4)6O2 – Pb2+\n2Y8(SiO4)6O2;
Ca10(PO4)6(OH)2 – Ca4Y6(SiO4)6(OH)2;
M10(PO4)6F2 – M10(PO4)6F2 (M = Sr, Ba, Pb);
M10(PO4)6F2 – M10(MnO4)6F2 (M = Sr, Ba, Pb).
Since apatite is an important accessory mineral in most common rock types, it is often used in trace element and isotope investigations of igneous and metamorphic rocks [123]. Stable isotope compositions of biologically precipitated apatite in bone, teeth and scales are widely used to obtain the information on the diet, behavior and physiology of extinct organisms and to reconstruct past climate in terrestrial and marine conditions [124].
\nBroad spectrum of substitutions in the apatite lattice allows the incorporation of various isotopes, which offer a number of instruments for the interpretation of paleoenvironment and diagenesis. The relative stability of francolite compared to other sedimentary minerals led to an enormous number of studies and applications. Various isotopes occupy the Ca2+ and PO43− sites in the lattice of apatite (Fig. 16).
\nPossible isotopic substitutions in the structure of francolite [125].
Since the earliest application in deep-time study of Late Cretaceous paleotemperatures in 1950, the oxygen isotope paleothermometry is based on the temperature dependence of oxygen isotope fractionation between authigenic minerals[1] - [126] and ambient waters. Under the equilibrium conditions, the 18O/16O ratio of sedimentary carbonate and phosphate minerals depends only on the temperature of precipitation and on the 18O/16O ratio of ambient water. Thermodynamic relationships and bond vibrational frequencies can be used to determine the mineral-water isotopic fractionation relations but not with the precision and accuracy necessary for the paleothermometry. Such an application requires the calibrations based on mineral-water oxygen exchange experiments at high temperatures, mineral precipitation experiments at low temperatures and/or natural experiments using minerals grown under known conditions [127],[128].
\nCarbon, oxygen and sulfur isotopes are used to reconstruct the oxygenation stages of the sediments during organic matter degradation and precipitation of apatite. The application of this method gives good results for modern and Neogene deposits. In older occurrences, the signature of carbon and oxygen composition is commonly overprinted by diagenetic and burial diagenesis [125],[129]. The carbon isotope ratios of apatite can be used to interpret the source of carbon in magmas and metamorphic fluids using the assumption that the carbon isotope fractionations between phases are small in igneous and metamorphic systems [123].
\nThe carbon isotope analysis of bioapatites was first applied to terrestrial mammals in early 1980s [130],[131],[132]. While it is now known that some bones do undergo the C-isotope exchange extremely readily, collagen, bone and enamel record different periods of time during the life of a single individual, and the diet may change. That means, there is a fundamental ambiguity (preservation vs. normal intraindividual differences) in interpreting the isotopic differences among different tissues. Unfortunately, early results were taken to imply that all bioapatites are unreliable, and it was not until the 1990s that it became accepted that the tooth enamel, at least, is a robust recorder of diet. Thus, the early work of
Fossil biogenic apatites display the trace element compositions that can record environmental and biological signals, give insights into past water compositions or be used for dating paleontological and archeological bones and teeth. The mechanisms of the process of trace element and their isotopes incorporation into apatites of skeletal phosphatic tissues are described by
Partitioning between aqueous fluids and crystals;
Surface adsorption, complexation and chelation;
Diffusion processes.
Partitioning of divalent cations is defined by the chemical equilibrium expressing the divalent cation (Me2+) exchange between apatite and aqueous solutions [135]:
where (aq) and (ss) refer to the aqueous solution and to the solid solution, respectively. The equilibrium constant of Eq. 31 can be written as
where x is the molar fraction in apatite solid solution, m is the molality in water, λ is the activity coefficient of the component in the solid solution, K(T) is the solubility product of the end-member at temperature T and γ is the ion activity in the aqueous solution, the ratio of which in water is assumed to be equal to one. The activity coefficients in regular solid-solution model are described by Margules parameters[1] - [136] and can be approximated by the elastic energy due to the deformation of the host crystal lattice around the substituted cation [135],[137]:
where NA is the Avogadro number, E is the Young’s modulus of the crystal, ri is the ionic radius of cation normally occupying the site in the i-compound (Ca in apatite) and rj is the ionic radius of the substituted cation in compound j. The elasticity of hydroxyapatite gives E = 114 ± 2 GPa.
\nAt low concentrations (XMe−apatite << 1) like those of trace elements in biogenic apatites, Eq. 32 is reduced to the relationships [135]:
where the term exp (-ΔGideal/RT) is the free enthalpy change of the reaction 31, equivalent to the ratio of end-member solubility products. Unlike carbonates, the data of solubility products and thermodynamics for end-member apatites are scarce. When no data are available for the solubility and enthalpy of formation of the end-members, it is assumed that the elastic energy term dominates over the partitioning, i.e. ΔGideal ≪ WGMeCa. Promising ways for obtaining the enthalpies of formation and the substitution energies are the first-principle calculations [138] and the atomistic modeling [135],[139].
\nFor heterovalent substitutions, the equilibrium reaction becomes complex since complementary substitutions are necessary to maintain the charge balance in the crystal. Typically, the substitution of trivalent elements of important rare-earth series requires the compensation by Na+ for Ca2+ at an adjacent site or even more complex substitution scheme involving carbonate groups or fluorine. In that case, most thermodynamic data required for the calculation of the equilibrium constant are not available. Among the series of elements with the same charge and substitution scheme, the pattern of equilibrium constants, or of distribution coefficients, can be approximated by combining Eqs. 33 and 34 [135]:
where Eeff is the effective Young’s modulus and r0 is the optimum radius for maximum equilibrium constant KD0, all of which will depend on the charge of the considered series of elements. These parameters can be adjusted to experimental data such as partition coefficients between minerals and liquids and lead to parabola-like curves, the position and curvature of which depend on the charge of the element. This approach was applied so far only to rare-earth elements in apatite, where the relative partition coefficients were extrapolated from magmatic temperatures around 800°C to low temperatures appropriate for fossil diagenesis [135].
\nThe complexation of metal cations in aqueous fluids involves binding with a broad range of molecules from simple inorganic ones (e.g. carbonates, phosphates and sulfates) to complex organic ones (humic acids, amino acids, proteins, enzymes, etc.). For molecules with several bonding sites and structural flexibility (e.g. multidentate or chelator), the complexation is thermodynamically favored with respect to the complexation with several monodentates having one bonding site; the process is named chelation. Chelators can be adsorbed on mineral surfaces while remaining complexed to metallic cations. The pattern of the partition coefficients associated with this process was measured for rare-earth elements complexed with humic acids and manganese oxides. It shows null fractionation along the whole series; the effect of chelation is therefore to screen the trace element in the crystal or ligand field and to suppress the fractionation associated with ionic radius variations and tetrad effects, and most of the anomalies associated with redox of Ce [140]. Similar effects might occur for the adsorption of chelated metals on other mineral surfaces and in particular phosphates. In addition to chelators, the transition metals also form complexes with proteins and enzymes that interact with bones and teeth in living organisms and may influence their incorporation in bioapatite [135].
\nSolid-state diffusion in crystals is a thermally activated process governed by the enthalpy of formation and of migration of defects and usually well described by the Arrhenius relation [135]:
where D0 is the pre-exponential factor corresponding to the diffusion coefficient at infinite temperature and ΔHa is the activation enthalpy (or energy) of the diffusion process. The extrapolation of high-temperature diffusion data of trace elements in apatite shows that these processes are inefficient at temperatures below 300°C, which cover the conditions of diagenetic alteration up to low-grade metamorphism [135],[141].
\nThe differing initial and boundary conditions imposed in three sets of diffusion experiments:
Ion implantation;
In-diffusion with powder sources experiment;
Out-diffusion.
consequently resulting in different solutions to the diffusion equation. However, in all cases, the process can be described as one-dimensional, concentration-independent diffusion [141].
\nThe summary of data diffusion for cations and anions in apatite (a) [142] and the diffusion of Sm and Nd for various minerals and oxides (a) [141].
A plot of diffusivities of various cations and anions in apatite is shown in Fig. 17(a). The diffusivities of Mn are similar to those of Sr and about an order of magnitude slower than those of Pb. On the other hand, the diffusion of Mn2+ in apatite is about two orders of magnitude faster than the diffusion of (trivalent) REE when coupled substitutions according to Eqs. 4 and 5 are involved [141],[142]. The diffusion coefficients of Nd and Sm in various minerals and related oxides are plotted in Fig. 17(b). The diffusion of REE in apatite is relatively fast; when only simple REE exchange is involved, it is among the fastest in rock-forming minerals for which the data exist. Even when the chemical diffusion involving coupled exchange is considered, REE transport in apatite is considerably faster than the REE diffusion in other accessory minerals [141].
\nKetamine is listed in the WHO Essential Medicines List since 1985 as an anaesthetic and analgesic. Unlike other commonly used anaesthetic agents, ketamine does not tend to cause respiratory depression or hypotension, making it ideal for use as a general sedative and in veterinary medicine [1].
\nHowever, ketamine is also a drug of abuse. The United Nation’s World Drug Report 2019 shows that ketamine has been the dominant hallucinogenic seized by authorities globally, accounting for 87% of such seizures in the past 5 years [2]. In 2017, the global quantity of ketamine seized was approximately 11,000 kilogrammes, the majority of which was in Asia [3]. Most ketamine seized, in the order of descending quantity, was reported by mainland China, followed by Taiwan, Hong Kong, Malaysia, Myanmar, Thailand, the United Kingdom, India, and the Netherlands [3]. In Taiwan, ketamine has been the most frequently abused illicit drug since 2006. The volume of seizures there grew from 916 kg in 2009 to 1187 in 2010 [4]. However, ketamine is becoming more and more popular not only in Southeast Asia but in Europe as well. The number of ketamine users in the United Kingdom grew from 85,000 in 2006 to 113,000 in 2008, becoming the fourth most popular illicit drug among UK clubbers [5]. Its popularity could be explained by its low market price among recreational drugs and also the difficulty in cracking down on its trafficking, as it is produced legally for medical use [6].
\nThe chronic and illicit use of ketamine is associated with urinary tract damages. Structural damage to the bladder, ureters, and kidneys has been demonstrated in numerous animal and human studies. Patients usually present to the urological service with symptoms such as urinary frequency, haematuria, and dysuria. Management is multidisciplinary, as a big part of treatment success lies not only in urological interventions but also in successful abstinence.
\nThe exact prevalence of ketamine-associated cystitis is difficult to ascertain, as most users are reluctant to seek medical attention despite symptoms. A study in Taiwan conducted in 2019 by Li et al. reported that whilst 84% of chronic ketamine abusers demonstrated urinary tract symptoms, only 48% sought treatment [7]. A survey involving 3806 participants in the United Kingdom by Winstock et al. found that 26.6% of ketamine users report urinary symptoms and that the symptoms are significantly related to both frequency and duration of use [8]. Similarly, Pal et al. from the United States conducted a survey involving 18,802 participants which reported a 30% prevalence of lower urinary tract symptoms (LUTS) among recent ketamine users [9].
\nLower urinary tract symptoms, as well as dysuria and haematuria, are the most common symptoms caused by chronic ketamine abuse. LUTS in the setting of ketamine cystitis usually comprises urinary frequency, feeling of incomplete bladder emptying, and nocturia. More than 50% of users complain of urinary frequency after using ketamine for about 2 years [7]. The severity and number of symptoms are correlated with not only the duration of use but also the route of administration. Ketamine may be cut up into a powder form before being inhaled or smoked with pipe-like devices. Snorting causes significantly more symptoms than smoking. This is possibly due to a higher amount of ketamine entering the circulation via the nasal mucosa [7].
\nThe combined use of ketamine with other substances such as marijuana and 3,4-methylenedioxy-methamphetamine (MDMA) has also been found to significantly increase the severity of LUTS. Marijuana enhances the expression of cannabinoid receptors CB1 and CB2, which are found in the human bladder urothelium [10]. This is implicated in the worsening of storage symptoms such as frequency and urgency. The mechanism through which MDMA exacerbates LUTS remains to be elucidated.
\nA number of mechanisms have been proposed to explain the pathogenic effects of ketamine on the urinary system. These include (1) direct toxicity of ketamine or its metabolites on the bladder tissues; (2) microvascular changes in the bladder and kidneys by ketamine or its metabolites; and (3) delayed (type IV) hypersensitivity against the urothelium due to ketamine or its metabolites [11]. Infection is unlikely to play a role in the primary pathogenesis of ketamine cystitis, as the vast majority of patients do not have a positive urine bacterial culture. As of yet, there has not been a single conclusive theory on the mechanism of ketamine-induced cystitis.
\nIn vitro studies on human urothelial cells have demonstrated dose-dependent toxicity of ketamine to human urothelial cells. The damage is carried out by both ketamine itself and its primary metabolite (norketamine) [12]. Norketamine is generated as ketamine undergoes hepatic metabolism. Both ketamine and norketamine are subsequently excreted in the urine. Ketamine and norketamine are equally toxic to the urothelium in in vitro studies, but norketamine remains in the urine for longer than ketamine, and hence norketamine may be accountable for more of the damage done [13]. As with other toxic exposures, daily exposure has been found to be more damaging than a one-off exposure. The accepted anaesthetic dosage of ketamine for human medical use is 0.5–2 mg/kg, but much higher concentrations are abused in recreational use (up to 20 g per day in some users) [13]. As aforementioned in the previous section, it also takes approximately 2 years of abuse before cystitis symptoms arise. Therefore, as ketamine is used at much lower doses as well as frequency in the context of anaesthesia as compared to daily abuse, the medical use of ketamine for one-off anaesthesia is less likely to cause significant ketamine cystitis.
\nThe hypothesis that ketamine and norketamine exert a direct effect on the urothelium is based on the knowledge that both chemicals are excreted by the urine and have a long contact time with the urothelium (ketamine 5 days, norketamine 6 days) after ingestion [14].
\nThe urinary tract from the renal pelvis to the proximal urethra is covered by the urothelium, a highly specialised transitional epithelium capable of stretching to accommodate various degrees of distension in response to urine volume. The urothelium comprises three layers—superficial, intermediate, and basal. Under the urothelium lies the submucosa, then the detrusor muscle, and then the adventitia.
\nClassic histological changes found in ketamine cystitis include denudation of the urothelium, as well as inflammatory changes including oedematous vessels, and infiltration by eosinophils and T-lymphocytes [15]. The affected urothelium loses its superficial layer (which provides a barrier function), thus exposing the stroma to further insults from urinary ketamine and norketamine. This may be one of the mechanisms by which ketamine causes cystitis and the resultant symptoms. Some of these histological changes are similarly seen in interstitial cystitis (chronic bladder pain in the absence of an identifiable aetiology) [16]. Additionally, haematoxylin and eosin staining in the urothelium affected by ketamine cystitis may in some cases display apparent dysplastic changes with the loss of epithelial cohesion. Such changes mimic the histology of carcinoma in situ, and hence the clinical history of ketamine abuse should alert the clinician or pathologist to the possibility of misdiagnosis of carcinoma in situ [12].
\nThe infiltration by T-lymphocytes suggests that a delayed (type IV) hypersensitivity reaction to ketamine may also play a role in the pathogenesis of ketamine cystitis [17]. This is because T-lymphocytes are heavily implicated in type IV hypersensitivity reaction, and it is known that type IV hypersensitivity reactions occur only after prolonged exposure to the causative agent. This reaction conforms to the temporal profile of the development of ketamine cystitis, where symptoms usually develop only after 2 years of abuse.
\nThe irritative effects of ketamine on the urinary system, especially the bladder, produce myriad symptoms. These include:
Urinary frequency
Feeling of incomplete bladder emptying
Nocturia
Urinary urgency
Urge incontinence
Haematuria
Suprapubic pain or ‘bladder pain’
The typical complaint from the affected patients is ‘painful, small voids’, closely mimicking that of interstitial cystitis. These symptoms typically develop after 2 years of ketamine abuse. A study in Hong Kong by Ng et al. has demonstrated the relative prevalence of symptoms as follows: urgency (92%), frequency (84%), nocturia (88%), dysuria (86%), and haematuria (68%) [18]. The most bothersome symptoms reported by users are typically urinary frequency, nocturia, and urgency. This is because of the need of frequency visits to the bathroom, which interferes significantly with their daily activities [7].
\nThe clinician may evaluate symptoms using standardised methods such as frequency-voiding charts (also known as a ‘bladder diary’) and questionnaires such as the Pelvic Pain and Urgency/Frequency (PUF). A frequency-voiding chart involves the patient recording the volume of every fluid intake and void and also instances and degrees of urge incontinence, if any. Reviewing a frequency-voiding chart allows the patient to communicate effectively with the clinician the frequency and nocturia experienced. Ketamine cystitis typically produces a low-compliance bladder, manifesting as frequency, low-volume voids. Urge incontinence is the sudden and compelling desire to pass urine that is difficult to defer and is accompanied by involuntary leakage.
\nThe Pelvic Pain and Urgency/Frequency questionnaire is a symptom score questionnaire developed and validated for the diagnosis of interstitial cystitis [19]. As mentioned, interstitial cystitis produces symptoms and histological changes in the bladder akin to those found in ketamine cystitis, and studies have validated the use of this questionnaire to score patients experiencing symptoms of ketamine cystitis [18]. The questionnaire includes eight questions evaluating daytime frequency, nocturia, pelvic pain, urinary urgency, the degree to which these symptoms bother the patient, and sexual function. PUF generates a symptom score and bother score, which total at 35. In a patient with history of significant ketamine abuse, a score of ≥15 indicates the presence of significant cystitis symptoms, thus leading to the diagnosis of ketamine cystitis. The PUF is a useful tool not only for the diagnosis of ketamine cystitis but also for symptom quantification so that its severity and response to treatment could be monitored over time.
\nCystoscopy, computed tomography (CT), ultrasonography, and pyelography are examples of investigations that may demonstrate the structural damage implicated in ketamine cystitis [20]. Cystoscopy reveals inflammatory changes such as telangiectasia (indicative of neovascularisation), ulceration, or even petechial haemorrhage in severe cases. Biopsies of the affected bladder urothelium will reveal histological changes mentioned earlier in the chapter, including denuded epithelium and infiltration by eosinophils and lymphocytes. Computed tomography may show bladder wall thickening and peri-vesical stranding, both of which are indicative of chronic inflammation of the bladder wall (\nFigure 1\n). Upper tract damage usually manifests itself as unilateral or bilateral hydronephrosis, with ureteric wall thickening, or luminal narrowing and strictures. CT, pyelography, and ultrasound are all suitable modalities to demonstrate hydronephrosis (\nFigures 2\n–\n4\n). CT and pyelography have the additional benefit of evaluating the exact level of ureteric stricturing.
\nContrast CT scan image showing a thickened and contracted bladder in a patient with a 7-year history of ketamine abuse.
Reconstructed contrast CT urogram showing bilateral hydronephrosis and hydroureter down to the level of the vesicoureteric junctions. The bladder also appears small with generalised wall thickening. This patient has an 8-year history of ketamine abuse.
This is an antegrade pyelogram of a patient suffering from ketamine cystitis. Contrast is injected through the percutaneous nephrostomy. There is hydronephrosis and a contrast upholding at the level of the L3 vertebra. This is suggestive of a ureteric stricture at that level causing hydronephrosis.
Ultrasound image of the left kidney of a patient with ketamine cystitis complicated by acute left pyelonephritis. This patient had a background of ketamine cystitis with bilateral hydronephrosis. She presented acutely with left loin pain and fever. The ultrasound image shows debris in the chronically dilated renal pelvis. This is compatible with acute pyelonephritis complicating ketamine cystitis. A combination of chronic obstruction and vesicoureteral reflux has likely contributed to the development of upper tract infection.
Apart from assessing the degree of structural damage, the functional capacity of the urinary system should also be assessed. Urodynamic studies, such as video cystometrogram, reveal reduced bladder capacities, reduced bladder compliance, and sometimes detrusor overactivity even at low bladder volumes. Bladder capacities of ketamine cystitis patients are typically <150 ml, and detrusor overactivity has been shown to be evident at bladder volumes as low as 14 ml [21]. This means that such patients will not only complain of very frequent but small voids, they are also likely to experience urge incontinence. One can see how disabling such symptoms are from these investigation findings (\nFigures 5\n–\n7\n).
\nCystometrogram (filling phase) of a patient with a 10-year history of ketamine abuse. First desire to void was recorded at 14 ml of bladder filling. Also note the multiple spikes at the lowermost tracing indicative of detrusor overactivity. (Pves, intravesical pressure; Pabd, intra-abdominal pressure; Pdet, subtracted detrusor pressure of Pves–Pabd).
Cystometrogram (filling phase) of the same patient after 3 years of abstinence. First desire to void at 51 ml. Note the difference in the scale of the x-axis denoting volume. The detrusor overactivity has also dampened, as shown by the smoother Pdet tracing.
Cystometrogram (filling phase) of the same patient after 8 years of abstinence. First desire to void at 75 ml. Much improved bladder compliance as shown by the relatively smooth Pdet tracing.
Renal impairment can be reflected from raised serum creatinine or impaired creatinine clearance and estimated glomerular filtration rate. Renal impairment may stem from vesicoureteral reflux (VUR) due to chronic reduction in bladder compliance. VUR can be demonstrated on video cystometrogram as a reflux of contrast material from the bladder up to the ureters. VUR predisposes the upper tract from urinary tract infections, increasing the risk of recurrent pyelonephritis and resultant renal scarring (\nFigure 2\n). Hydronephrosis as a result of ureteric narrowing is also a cause of renal impairment in these patients. Ureteric narrowing is likely secondary to urinary ketamine and its metabolites causing transmural inflammation and swelling or even fibrosis and strictures (\nFigure 8\n).
\nContrast CT scan image of a patient with more than 3 years of ketamine abuse, showing bilateral atrophic kidneys and hydronephrosis. This patient required bilateral percutaneous nephrostomies (also seen on this image) for upper tract urinary diversion.
Papillary necrosis may be seen on renal ultrasound or on contrast studies such as an intravenous urogram or computed tomography [11]. The contrast material fills necrotic cavities located in the renal papillae. Sometimes, sloughed necrotic material may pass into the ureter, causing obstruction, and appear as a filling defect.
\nThe management of ketamine cystitis aims at abating the debilitating urinary symptoms and preventing further damage to the urinary tract. The most important components of the management plan therefore lie in early diagnosis and early abstinence, as this aims to effectively remove ketamine and its metabolites from the urinary system before irreparable damage to the urinary system sets in. A large-scale study involving more than 1000 ketamine users reported that up to 50% of users report symptomatic improvement after cessation of use. Urinary frequency has been shown to be the first symptom to improve [8]. That said, as with any detoxification program, psychosocial challenges pose a big barrier to long-term abstinence. It is therefore imperative that the clinician solicits help from relevant parties such as social workers, clinical psychologists, or even psychiatrists to form a multidisciplinary approach in managing these patients [22]. This process involves first identifying those suffering from ketamine cystitis, then explaining the relationship between ketamine use and cystitis, and finally embarking on the detoxification journey. As mentioned earlier in the chapter, the PUF scale serves as a standardised and validated means of identifying ketamine users suffering from cystitis. Success in multidisciplinary management has been demonstrated by outreach teams comprising urologists, psychiatrists, social workers, and nurses in Hong Kong [23].
\nAlthough the precise mechanism of injury in ketamine cystitis has yet to be elucidated, it is clear that it involves inflammation of the urothelium akin to that of interstitial cystitis. Medications that aim to reduce inflammation, such as nonsteroidal anti-inflammatory drugs (NSAIDs) and glucocorticoids, have thus been studied in the treatment of ketamine cystitis symptoms. Other treatment regimens involving the use of antibiotics, anti-muscarinic agents, and beta-3 agonists have also been examined. However, the results from the medication therapy have been suboptimal overall [24].
\nMedication therapy may not result in significant improvements in LUTS for these patients, but analgesics should still be employed generously. This is because ketamine itself possesses analgesic properties, and therefore abstinence after long periods of abuse may produce pain akin to a withdrawal effect. Analgesics such as paracetamol, phenazopyridine, or even narcotic analgesics such as tramadol may be used on top of NSAIDs in high doses as pain relief during the initial period of detoxification [25].
\nKetamine and its metabolites cause denudation of the urothelium, exposing the underlying submucosa and stroma of the bladder wall to further toxic damage. This produces the typical LUTS as well as the structural changes such as wall thickening and reduction in compliance. This has prompted investigations into the effectiveness of intravesical therapies that aim to restore the integrity of the urothelium so that the underlying tissue may no longer be exposed to the toxicities of ketamine and its metabolites. Intravesical instillation of a glycosaminoglycan, such as hyaluronic acid or chondroitin sulphate, has been proposed to reconstitute the barrier function provided by the urothelium and enhance healing. Reports of significant reductions in symptoms in patients treated with weekly intravesical instillations of hyaluronic acid or chondroitin sulphate have been published recently [26]. These patients not only reported a reduction of LUTS, but follow-up cystoscopy with biopsies showed decreased inflammatory cell infiltration, less inflammatory hypervascularity, as well as regeneration of the urothelium [27].
\nCystoscopic injection of botulinum toxin into the bladder wall, followed by hydrodistension, is another intravesical treatment that has been shown to relieve symptoms of ketamine cystitis [28]. Botulinum toxin type A inhibits the presynaptic release of neurotransmitters such as acetylcholine, thus inactivating neuromuscular junctions and reducing detrusor activity. The patient is typically put under spinal anaesthesia, and a cystoscope is then advanced into the bladder. 20 ml of botulinum toxin type A at a concentration of 200 IU in 20 ml is then injected into 40 points in the bladder wall. There is currently no standard protocol for the technique of hydrodistension, but authors have performed it by filling the bladder with saline under a pressure of 80 cmH2O, at a volume of 150–200 ml, for a duration of 5 minutes [29].
\nThe bladder in a patient with severe ketamine cystitis is thickened and fibrotic and has poor compliance. Apart from severe LUTS, these changes may also cause vesicoureteral reflux and upper tract damage. Such patients are at risk of chronic renal failure. Surgical treatment in the form of augmentation cystoplasty is therefore an option to increase the capacity and compliance of the bladder, so that symptomatic improvement and upper tract protection could be brought about through a single procedure. Techniques vary, but an option is to use a 25 cm segment of the ileum and sew it to a surgically created clam-like opening of the bladder in order to augment its volume and compliance [30]. Contraindications to augmentation cystoplasty using bowel include any condition that renders the bowel abnormal at the baseline, for example, inflammatory bowel disease (Crohn’s disease, ulcerative colitis) and previous gut resection (such that further resection may predispose the patient to malabsorption or even short gut syndrome). Another alternative is to use a portion of the stomach, termed gastrocystoplasty. This has its own issues, as the hydrochloric acid produced by the stomach mucosa may cause haematuria-dysuria syndrome, peptic ulceration in the bladder, and alkalosis. Complications include a mortality rate of up to 2.7%, small bowel obstruction, fistulation, and renal failure (due to the reabsorption of urinary waste through the bowel segment). Some patients may furthermore require clean intermittent catheterisation to more effectively empty the bladder. Patient selection is paramount when considering augmentation cystoplasty for ketamine cystitis patients. Failure of abstinence after surgery results in rapid reabsorption of ketamine from the urine through the bowel segment. Ketamine and its metabolites are hence recirculated, excreted in the urine again, and once again exerting their toxic effects on the urothelium. Augmentation cystoplasty with bowel may therefore even accelerate upper tract damage should the patient fail to abstain from ketamine postoperatively. The patient should also be willing to comply with clean intermittent self-catheterisation should it be required [30].
\nAn alternative surgical strategy is an ileal conduit [31]. This involves brining both the ureters to an opening in the abdominal wall through a surgically created segment of the ileum. This obviates the need for clean intermittent catheterisation and offers quicker postoperative recovery. However, as this is an incontinent type of urinary diversion, the patient would have to live with a lifelong urostomy bag.
\nSome patients present with bilateral hydronephrosis with or without impairment of renal function. This could be due to vesicoureteral reflux or ureteric strictures. As most patients with ketamine cystitis are young, it is of paramount importance that their upper tract is protected to prevent chronic renal disease. Methods to achieve this include percutaneous nephrostomy and ureteral stenting. Percutaneous nephrostomy involves placing a plastic tube through the skin into the renal pelvis so that the urine produced by the kidney may drain through the tube into an external bag instead of being trapped in the obstructed system. The drainage of the urine through nephrostomy tubes into an external bag also reduces the LUTS from ketamine cystitis, as there is significantly less urine entering the bladder. Disadvantages include inconvenience, as well as nephrostomy tube-related complications such as frequent dislodgement, and blockage. The inconvenience associated with the use of a nephrostomy tube is due not only to the presence of the tube exiting the loin but also to the bag to which it is connected. Another way of ensuring upper tract drainage is by retrograde stenting [32]. Double J stents can be inserted via a cystoscope to ensure ureteric patency. This method obviates the need for external tubes and bags, but as urine is allowed to flow into the bladder, LUTS may persist. Additionally, some patients may also suffer from stent symptoms, which include LUTS due to the stent tips in the bladder irritating the urothelium.
\nUrologists in Hong Kong such as Ma et al. have established a clinical pathway in order to guide and standardise the management of ketamine cystitis [22]. Patients going through such a clinical pathway will receive a full workup of the extent of their ketamine cystitis and complications and receive treatment accordingly (\nFigure 9\n).
\nClinical pathway for the management of ketamine cystitis (adapted from Ma et al.) [22].
The treatment of ketamine cystitis revolves heavily around abstinence. However, addiction and withdrawal symptoms, as well as the socioeconomic factors that contribute to the persistence of ketamine abuse, are not the only factors that hamper successful abstinence.
\nAbstinence from ketamine in the presence of ketamine cystitis is made more difficult by bladder pain and dysuria. As ketamine exhibits analgesic effects, it paradoxically suppresses the bladder pain and dysuria caused by ketamine cystitis. Subsequently, the cessation of ketamine use will unmask more intense cystitis symptoms. If such symptoms are inadequately controlled by more effective analgesics, the patient may be driven to use ketamine as a means to control the cystitis symptoms. Such a pattern of abstinence, failure of symptomatic control, and relapse creates a vicious cycle. It is therefore important to prescribe the patient with adequate analgesia according to the analgesic ladder to effectively suppress bladder pain and dysuria. The flip side of this is that the patient may in turn become dependent on the prescribed analgesics, especially if opioids are used [25].
\nFailure of abstinence in patients who have received surgical treatment such as augmentation cystoplasty may prove to be detrimental. As mentioned in the Management section, the reabsorption of ketamine and its urinary metabolites via the bowel segment used for augmentation cystoplasty may accelerate damage to the upper urinary tract, making the surgical treatment counterproductive. Correct patient selection for surgical treatment weighs heavily upon the urologist [31].
\nUpper tract protection by means of bilateral percutaneous nephrostomies (PCNs) may be the last resort for patients with identifiable hydronephrosis and impaired renal function [33]. However, as most ketamine cystitis patients are young and ambulatory, bilateral PCNs prove to be a cumbersome and a general nuisance. Not only are the nephrostomy tubes and bags inconvenient to live with, they also come with issues such as dislodgement or tube blockage. Tube-related issues may require hospitalisation for the revision of the nephrostomies, which adds not only to patient dissatisfaction but also to overall healthcare costs. With such inconvenience, the patient may be deterred from complying with having bilateral PCNs and in turn exposes himself to risks of chronic kidney disease and eventual dialysis dependence. Dialysis dependence in this age group makes the employment difficult, which then contributes to a lack of socioeconomic support and again makes abstinence a challenge.
\nLong-term ketamine abuse leads to the development of ketamine cystitis. Symptoms are debilitating and interfere significantly with the patient’s daily activities. Furthermore, the upper tract may also suffer from irreversible damage, such as ureteric stricturing and finally chronic renal failure. Management of ketamine cystitis starts with its identification. This could be achieved using standardised symptom score questionnaires in known abusers of ketamine. Investigations such as blood tests, computed tomography, and cystometrogram are useful to characterise and delineate the extent of ketamine cystitis and its sequelae. The cornerstone of effective treatment is abstinence. This is done via a multidisciplinary approach involving urologists, psychiatrists, social workers, and other relevant disciplines. Intravesical therapies, such as hyaluronic acid instillation and botulinum toxin injection, are emerging options that have shown promising results. Upper tract protection in the form of long-term percutaneous nephrostomies may save the patient from suffering from chronic renal failure.
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