",isbn:"978-1-83969-164-5",printIsbn:"978-1-83969-163-8",pdfIsbn:"978-1-83969-165-2",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!0,hash:"918540a77975243ee748770aea1f4af2",bookSignature:"Dr. Aakash Goyal",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/9651.jpg",keywords:"GWAS, Cereals, Breeding, Disease Resistance, Wheat, Rice, Maize, Drought Tolerance, Genetics, Production, Quality, Yield",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"October 21st 2020",dateEndSecondStepPublish:"December 4th 2020",dateEndThirdStepPublish:"February 2nd 2021",dateEndFourthStepPublish:"April 23rd 2021",dateEndFifthStepPublish:"June 22nd 2021",remainingDaysToSecondStep:"a month",secondStepPassed:!0,currentStepOfPublishingProcess:3,editedByType:null,kuFlag:!1,biosketch:"Elected fellow member of the International College of Nutrition (FICN) and Society of Applied Biotechnology (FSAB) with research experience at Agriculture and Agri-Food Canada, Bayer Crop Science, ICARDA, InnoTech Alberta, and Palm Gardens Inc.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"97604",title:"Dr.",name:"Aakash",middleName:null,surname:"Goyal",slug:"aakash-goyal",fullName:"Aakash Goyal",profilePictureURL:"https://mts.intechopen.com/storage/users/97604/images/system/97604.jpg",biography:"Aakash Goyal was born in India, and graduated from MDU, Ajmer (Biology) in 1999, then obtained Master’s in Biotechnology in 2002 from GJU, Hissar specialization in Plant biotechnology & molecular breeding, and PhD. in Genetics and Plant Breeding in 2007 from CCSU, Meerut India, specialization in Wheat Breeding. After completion of PhD, he obtained NSREC Visiting Fellowship (in 2008) and thus, joined the wheat and triticale breeding program at Lethbridge Research Center, Agriculture and Agri Food Canada (AAFC), Lethbridge, AB., Canada. In 2012, he achieved a position as a Wheat Breeder for Bayer Crop Science, Saskatoon, Canada. In 2014 he had the honor to obtain Senior Research Scientist position with International Center of Agriculture Research in Dry Areas (ICARDA). In 2017, he moved back to Canada and joined as Native Plant Research Scientist with InnoTech Alberta. In November 2019 he joined as an Agriculture Specialist with Palm Gardens Inc. to help in breeding and cultivation of Cannabis. In this time (2002-2020), he has published nine Books and 50 research papers, reviewed articles, book chapters and book reviews. He is also an elected fellow member of International College of Nutrition (FICN) and Society of Applied Biotechnology (FSAB).",institutionString:"Palm Gardens Inc. 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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. 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\n
1. Introduction
\n
Whiteware is a traditional ceramic material used to make pottery and porcelain. Traditional raw material mixture for whiteware (porcelain) production covers kaolin or/and kaolin clay, quartz and feldspar rock at a composition about 50:25:25 wt.%. Typical properties of porcelain body are low porosity (below 0.3%), high mechanical strength (bending strength over 40 MPa, Young Modulus over 60 GPa), firing temperature about 1300°C and high whiteness and translucency [1, 2, 3].
\n
Feldspar rocks are used in the fine ceramic industry as a fluxing agent to form a glassy phase for accelerating of sintering process. Feldspar rocks are a mixture of pure feldspars, quartz and mica especially from the mineralogical point of view. Pure feldspars are divided into potassium feldspars (orthoclase, microcline), sodium feldspars (albite) and calcium feldspars (anorthite). Solid solutions between K‐feldspar and albite are called alkali feldspars, and solid solutions between albite and anorthite are plagioclase feldspars. The plagioclase series follows according to percentage of anorthite in parentheses [4]. Feldspar rocks are usually used as a source of alkali oxides (Na2O, K2O) and alumina (Al2O3)for the preparation of glazes [5]. Suitable choice of feldspar rock can significantly affect the properties of the ceramic body [6], firing temperature and soaking time [10]. The densification of green body, cleanability and the stain resistance of polished sintered ceramic tiles is influenced by particle size distribution of used feldspar rocks [7]. Feldspar rocks may be successfully replaced by LCD waste glass [8]. Wollastonite is very suitable material for acceleration of sintering process in porcelain body. Only 1 wt.% addition of wollastonite is able to decrease firing temperature (about 25°C) in the mixture with kaolin, quartz and potassium feldspar rock [9].
\n
Bone ash is fluxing agent for artistic porcelain especially known as bone china. The amount of bone ash in the raw material mixture of bone china is about 50% [11]. Bone ash (cattle bones calcined at around 1000°C) consists predominantly of hydroxyapatite. The reactions of bone ash in porcelain body were studied in detail in Refs. [12, 13]. Bone ash—fluxing agent for bone porcelains (bone china)—is usually produced by the calcination of bovine bones at the temperature of 1100°C. The melting point of bone ash is about 1670°C [14]. The mineralogical composition of bone ash consists of tricalcium phosphate in the form of hydroxyapatite Ca5(OH)(PO4)3.
\n
Very useful fluxing agent for sintered ceramic body production is zeolite, which is able to accelerate the sintering process very intensively. Zeolite is a natural mineral with exceptional physical properties that follow from its specific crystal structure. The latter consists of a 3D lattice of silicate tetrahedrons (SiO4)4− mutually connected by oxygen atoms, with part of silicon atoms replaced by aluminum atoms (AlO4)5−. Zeolite has a wide range of applications in agriculture, breeding, civil engineering, protection of environment, wastewater purification, and in various industrial sectors. In civil engineering, it began to be used as a partial replacement of cement in the production of concrete [15, 16, 17, 18, 19]. Different Italian low‐cost natural zeolitic rocks as a substitute of feldspar rocks in porcelain raw materials mixture were investigated. Zeolitic rocks increased the slip viscosity during wet grinding with a coarser grain size distribution. The technological properties (strength, porosity, resistance etc.) of zeolite‐based porcelain bodies are similar to current traditional porcelain bodies made in the system kaolin—feldspar rock—quartz [20]. The aim of the study [21] was to investigate the effect of natural zeolite addition on the sintering kinetics. Clinoptilolite, which is a type of natural zeolite, was added partially or fully in replacement of quartz at selected electro‐porcelain composition. It was found that the sintering activation energy decreased with increasing zeolite addition. Replacement of quartz with zeolite decreases activation energy for the start of sintering process in electro‐porcelain body—firing temperature (about 50–100°C) and soaking time were reduced. In the study [22], the effect of natural zeolite addition on the electrical properties of porcelain bodies was investigated. The resistivity of samples increased at 50°C temperature after zeolite addition, while it was decreasing after zeolite addition at higher temperatures. The resistivity of samples depends on sintering temperature. Low‐cost naturally occurring mixtures of feldspar and zeolite occurring in epiclastic rocks were promising substitutes for conventional quartz‐feldspathic fluxes in ceramic bodies. Different epiclastic outcrops, with a different zeolite‐to‐feldspar ratio, were tested in porcelain stoneware bodies. The addition of an epiclastic rock (20 wt.%) brought significant advantages (better grind ability, lower firing temperature with improved mechanical strength and lower porosity) and disadvantages (increasing of slip viscosity, worse powder compressibility, higher firing shrinkage, and a darker color of the body due to high amounts of Fe2O3) [23, 24].
\n
Anorthite type of whiteware body on the basis of raw materials mixture of feldspar rock, quartz and calcium aluminate cement (CAC) was developed at the firing temperature of 1300°C. Calcium aluminate cement (substitution of traditional kaolin or quartz) increases the strength of green body (\nFigure 1\n) and lowers the density due to formation of anorthite in all the fired bodies. An optimal ratio between quartz and feldspar rock for optimal sintering of the body was found (\nFigure 2\n) [25].
\n
Figure 1.
Variation of flexural strength of green body with hydration time. F, feldspar; Q, quartz; A, calcium aluminate cement (CAC) [25].
\n
Figure 2.
Water adsorption with various compositions in fired bodies with 20% of CAC [25].
\n
Whiteware body based on anorthite was developed from the mixture of ball clay, alumina, quartz, wollastonite and magnesia mixture. Sintered whiteware body (1220°C) has approximately two times higher modulus of rupture (110 MPa) than traditional porcelain body based on mullite due to lower content of glassy phase (only 30% for anorthitic whiteware body) [26]. Deflocculation of raw materials mixture based on calcium aluminate cement for the production of whiteware body with low porosity is necessary [27]. Carboxylic acids [28], polyethylene glycol, polyacrylate derivatives and aqueous solutions of sodium carboxylate [29] for optimalization of rheological properties of aluminous cement pastes were tested.
\n
Direct sintering is very effective method how to decrease the energy consumption during the firing of porcelain. Direct sintering reduced total processing time by ~50% and also lowered the sintering temperature from 1200 to 1175°C [30].
\n
For the description of sintering process, the thermodilatometrical analysis and sintering temperature are used primarily. Sintering temperature is defined as temperature when the fired body has water absorption exactly 2%.
\n
\n
\n
2. Sintering of whiteware body depending on fluxing agent (feldspar rocks, bone ash, zeolite)
\n
Sintering and melting of feldspar rocks depend on many aspects, such as the fineness of milling (granulometry), the rate of heating and finally the content of alkali oxides, because it directly creates the melting effect. Very useful is to compare the sintering activity of different typical feldspar rocks with different content of pure K‐feldspar, Na‐feldspar and Ca‐feldspar using for the industrial production of whitewares. The comparison is performed for pure feldspar rocks and for mixtures of feldspar rocks with kaolin. For the comparison, next feldspar rocks were used:
\n
Sodium‐potassium feldspar rock F‐KNa with mineralogical composition: K‐feldspar (microcline) 20.0%, Na‐feldspar (albite) 22.6%, Ca‐feldspar (anorthite) 2.4% and quartz 55.0%.
Potassium feldspar rock F‐K with mineralogical composition: K‐feldspar (microcline) 57.2%, Na‐feldspar (albite) 16.0%, Ca‐feldspar (anorthite) 1.5%, quartz 21.3% and mica (muscovite) 4.0%.
Sodium‐calcium feldspar rock F‐NaCa with mineralogical composition: Na‐feldspar (albite) 60.3%, Ca‐feldspar (anorthite) 21.0%, quartz 13.8% and mica (muscovite) 4.9%.
\n
The chemical composition of compared feldspar rocks (\nTable 1\n) reflects their mineralogical composition and volume of different types of pure feldspars (microcline, albite, anorthite). Granulometry of industrially milled feldspar rocks (the equivalent mean spherical diameter of particles d(0.5) in \nTable 1\n) is very similar and does not affect the presented results.
\n
\n
\n
\n
\n
\n
\n\n
\n
\n
F‐KNa
\n
F‐K
\n
F‐NaCa
\n
Zeolite
\n
\n\n\n
\n
SiO2\n
\n
79.76
\n
70.96
\n
66.67
\n
68.20
\n
\n
\n
Al2O3\n
\n
12.37
\n
16.10
\n
20.11
\n
12.40
\n
\n
\n
Fe2O3\n
\n
0.42
\n
0.10
\n
0.26
\n
1.40
\n
\n
\n
TiO2\n
\n
0.05
\n
0.04
\n
0.04
\n
–
\n
\n
\n
CaO
\n
0.48
\n
0.30
\n
4.23
\n
3.30
\n
\n
\n
MgO
\n
0.10
\n
0.06
\n
0.07
\n
1.00
\n
\n
\n
K2O
\n
3.35
\n
10.36
\n
0.83
\n
2.80
\n
\n
\n
Na2O
\n
2.67
\n
1.90
\n
7.13
\n
1.00
\n
\n
\n
LOI
\n
0.80
\n
0.20
\n
0.74
\n
–
\n
\n
\n
\nd(0.5) [μm]
\n
20.8
\n
18.4
\n
16.6
\n
20.0
\n
\n\n
Table 1.
Chemical composition of used feldspar rocks and zeolite in weight% (LOI = loss of ignition) and the equivalent mean spherical diameter d(0.5).
\n
Sintering activity of dry pressed test samples based on tested pure feldspar rocks (\nTable 1\n) was determined according to dependence of water absorption (EN ISO 10545) on the firing temperature (\nFigure 3\n). The most intensive sintering activity of the pure feldspar rock body shows potassium‐sodium feldspar rock F‐KNa—dry pressed test samples have the lowest water absorption, the highest bulk density and modulus of rupture in all firing temperatures in the range of firing at temperatures 1120–1210°C. Sodium‐calcium feldspar rock F‐NaCa begins sintering at much higher firing temperatures. Sintering temperature (\nFigure 3\n) of tested alkali feldspar rocks F‐KNa and F‐K is significantly lower than oligoclase type of feldspar rock F‐NaCa.
\n
Figure 3.
Water absorption E depending on the firing temperature. Determination of sintering temperature (E = 2%).
\n
The mixtures of feldspar rocks with kaolin (40 wt.%)—samples FK‐KNa, FK‐K, FK‐NaCa—totally change (increase) the sintering temperatures (\nTable 2\n) of alkali feldspar rocks F‐K and F‐KNa. The most intensive fluxing agent in case of pure feldspar rock body (F‐KNa) exhibits the lowest sintering activity in the mixture with kaolin with the highest sintering temperature. This fact is confirmed according to thermodilatometrical curves (\nFigure 4\n). Conversely, the mixture with kaolin decreases the sintering temperature of oligoclase F‐NaCa with the highest content of pure feldspars. The sintering temperature of F‐NaCa mixture with kaolin is lower (about 20°C) than pure feldspar rock F‐NaCa.
\n
Figure 4.
Thermodilatometric curves of pure feldspar rocks (F‐K, F‐KNa, F‐NaCa) and the mixtures of feldspar rocks with kaolin (FK‐K, FK‐KNa, FK‐NaCa) (10°C/min without soaking time on the maximal temperature).
\n
\n
\n
\n
\n
\n\n
\n
Mixture
\n
Sintering temperature (°C)
\n
Mixture
\n
Sintering temperature (°C)
\n
\n\n\n
\n
F‐K
\n
1205
\n
FK‐K
\n
1250 (+50)
\n
\n
\n
F‐NaCa
\n
1275
\n
FK‐NaCa
\n
1255 (−20)
\n
\n
\n
F‐KNa
\n
1190
\n
FK‐KNa
\n
1285 (+95)
\n
\n
\n
\n
\n
FK‐B
\n
1200
\n
\n\n
Table 2.
Sintering temperatures of tested samples based on different feldspar rocks and mixtures of kaolin (60%) with feldspar rocks (40%) or bone ash (FK‐B).
\n
The difference between the sintering of pure feldspar rocks (F‐KNa, F‐K, F‐NaCa) and mixtures of feldspar rocks with kaolin (FK‐KNa, FK‐K, FK‐NaCa) is evident from the thermodilatometrical curves (\nFigure 4\n). The highest content of quartz and muscovite in feldspar rock F‐KNa caused high expansion of the body during firing in the range of 200–900°C in comparison with other tested samples based on feldspar rocks F‐NaCa and F‐K. Dry pressed body based on pure feldspar rock F‐KNa shows the best sinterability of all compared feldspar rocks with maximal firing shrinkage (about 5%—\nFigure 4\n). Very significant is quartz transformation at the temperature 573°C on cooling part of thermodilatometrical curves (\nFigure 4\n) depending on quartz content (\nTable 1\n) in individual tested feldspar rocks. The quartz transformation is most visible for F‐KNa feldspar rock with maximal (55%) content of quartz.
\n
The feldspar rock F‐KNa with the lowest sintering temperature based on microcline and albite is typical by the quickest disappearing of feldspars during the sintering. Sintering temperature (1190°C) means the existence of only quartz and amorphous glassy phase without any feldspars (\nFigure 5\n). Quartz, amorphous glassy phase, and microcline are represented in the body F‐K after the firing at sintering temperature (1205°C). It is not possible to find an explanation of this fact in granulometry parameters of used feldspar rocks, which influence sintering and melting of feldspars very much, but in the equilibrium phase diagrams (\nFigure 6\n). Mixed sodium‐potassium feldspar rock generated low melting eutectic melts, which accelerate the sintering and melting process of feldspars. It is surprising that leucite generating during the potassium feldspars melting according to theoretical assumptions [4] is not detected even in sintered body F‐KNa or sintered body F‐K, both based on the potassium feldspar microcline. After the firing of F‐NaCa sample at sintering temperature (1275°C), the body contains anorthite (calcium feldspar) with high theoretical melting temperature of about 1550°C [4] and albite (\nFigure 5\n).
\n
Figure 5.
XRD patterns of sintered feldspar rocks at sintering temperature: M, microcline; Al, albite; Q, quartz; A, anorthite.
\n
Figure 6.
Phase diagram NaAlSi3O8—KalSi3O8—CaAl2Si2O8 and theoretical melting temperature of used feldspar rocks (1: F‐KNa, 2: F‐K, 3: F‐NaCa).
\n
The more intensive fluxing agent than feldspar rocks for the sintering process in the system kaolin‐fluxing agent is bone ash (\nFigure 4\n)—the mixture containing bone ash FK‐B (\nTable 2\n) shows sintering temperature 1200°C. That is about 50°C lower compared with the most intensive feldspar rock‐based mixture (FK‐K) with potassium feldspar rock F‐K containing 75% of pure microcline (\nTable 2\n). After the exceeding, the temperature 1200°C is visible intensive bloating of the bone ash bodies, which is typical by creating of secondary porosity and increasing in water absorption (\nFigure 4\n).
\n
Different mineralogical composition between feldspar rocks and bone ash‐based porcelain sintered bodies is possible to document according to XRD analyses. Traditional porcelain with high content of feldspar rocks in the raw materials mixture contains mullite and quartz as main mineralogical phases. Mineralogical composition of porcelain body based on bone ash is totally different—typical is high content of β‐tricalcium phosphate and anorthite. Bone ash in bone porcelain bodies decomposes into β‐tricalcium phosphate Ca3(PO4)2, lime CaO and water at around 775°C according to Eq. (1) [14]:
Eutectic composition in the ternary system of bone china (Ca3(PO4)2—CaAl2Si2O8—SiO2) is about 11% tricalcium phosphate, 51% anorthite and 38% silica with a melting temperature of 1290 ± 5°C [14].
\n
Zeolite rock was investigated as a fluxing agent for sintered ceramic body and its effect in the sintering process. The thermodilatometric heating and cooling curves dL/L0 of two different samples according to fluxing agent utilization (zeolite vs. feldspar rock F‐KNa) are shown in \nFigure 7\n. During the firing, there is evident (\nFigure 7\n) that zeolite (in mixture Z) is more intensive fluxing agent compared to feldspar rock F‐KNa (mixture F) for the creation of sintered body with low porosity. High firing shrinkage is typical for the sintering—the raw materials mixture not C, but Z with zeolite content starts intensive shrinking from temperature of about 900°C. Compared mixture F based on traditional ceramic fluxin agent - potassium feldspar rock F-K - starts the sintering process at a higher temperature (about 1100 °C).
\n
Figure 7.
Thermodilatometric analysis of compared samples with different fluxing agent (zeolite vs. feldspar rock F‐KNa) during the firing (5°C/min without soaking time).
\n
The quartz transformation at 573°C (change of the fired body volume) is visible on cooling part of thermodilatometric curve of the mixture F (\nFigure 7\n) due to high portion of quartz in the mixture F based on the mixture kaolin‐quartz‐feldspar. This phenomenon is not presented on the cooling curve of the sintered body Z based on zeolite—the raw material mixture not contains quartz, which is advantageous for lower relative expansion (coefficient of linear thermal expansion) of sintered body Z (\nFigure 7\n).
\n
Sintering temperature of tested samples based on zeolite is 1180°C, which is about 100°C lower than for the sample based on standard flux feldspar rock F‐K (mixture F). From the picture (\nFigure 7\n), there is evident different coefficient of linear thermal expansion α (in the temperature range of 30–500°C) of both compared sintered bodies (Z vs. F):
The sintered body based on zeolite shows the lower coefficient of thermal expansion α compared with feldspar sample due to the formation of anorthite in the sample Z and absence of quartz. Important technical property of anorthite is its low coefficient of linear thermal expansion of 48.2 × 10−6 K−1[31] (mullite 60 × 10−7 K−1 [32]). The mineralogical composition of both bodies after firing in both cases is characterized by the existence of mullite and glass phase. The sintered body (fired at 1200°C—mixture Z or 1300°C—mixture F, respectively) based on feldspar and quartz (mixture F) also contains quartz, and the body made from zeolite contains anorthite and cristobalite.
\n
Sintered body based on zeolite (mixture Z in \nFigure 8\n) as a fluxing agent not creates white body, which is typical for sintered body of the mixture F based on F‐KNa feldspar rock (\nFigure 8\n). This situation corresponds to chemical composition of natural zeolite with higher content of Fe2O3 (\nTable 1\n).
\n
Figure 8.
Color of sintered bodies with water absorption below 2%.
\n
\n
\n
3. The effect of calcium aluminate cement as a binder for the sintering of whiteware bodies
\n
The sintering process of whiteware (porcelain) body is affected by the used binder—we can use traditional plastic material (kaolin) or calcium aluminate cement (CAC) according to latest research [25, 33]. Comparison of the properties of both types (\nTable 3\n) of porcelains made by pressing from dry granulate is documented.
Composition of raw material mixtures (test samples).
\n
The difference in sintering process of two whiteware bodies with different binder kaolin vs. CAC (\nTable 3\n) is documented according to thermodilatometric curves (\nFigure 9\n). The sintering activity of both compared mixtures is very different when the firing temperature exceeds 1200°C—the system based on CAC (mixture CAC) is more able to sinter—we can observe higher firing shrinkage.
\n
Figure 9.
Thermodilatometric analysis of kaolin (K) and calcium aluminate cement (CAC)‐based bodies during the firing (1280°C, 3°C/min without soaking time). Determination of the coefficient of linear thermal expansion in the range of temperatures 30–500°C.
\n
Significant decrease of the coefficient of linear thermal expansion in the temperature range 30–500°C is evident (\nFigure 9\n) when calcium aluminate cement CAC is used as binder compared with kaolin based body. The explanation of this fact we can find in the formation of anorthite in the CAC‐based sample (\nFigure 10\n). The fired body based on kaolin also contains mullite and quartz as a main mineralogical phases. Anorthite exhibits lower coefficient of linear thermal expansion of 48.2 × 10−6 K−1 [31] than mullite 60 × 10−6 K−1 [32].
\n
Figure 10.
XRD of fired bodies based on different binder kaolin or CAC (M, mullite; Q, quartz; A, anorthite).
\n
The CAC mixture shows significantly higher sintering activity according to measured parameters of porosity—the prepared samples of a mixture CAC have a lower water absorption Ev and higher bulk density B (according to EN ISO 10545) than mixtures based on kaolin (K) after firing at the same temperature (\nTable 4\n). Higher modulus of rupture MOR of fired bodies is achieved for anorthitic type of body (CAC) compared with mullite whiteware body (K) when MOR values for samples with similar porosity are compared (K‐1280°C and CAC‐1250°C in \nTable 4\n). Similar results are published in Ref. [25].
\n
\n
\n
\n
\n
\n
\n
\n
\n\n
\n
Sample
\n
Firing temperature (°C)
\n
\n
\n
\n1250\n
\n
\n1280\n
\n
\n
\n
Ev (%)
\n
MOR (MPa)
\n
B (kg m−3]
\n
Ev (%)
\n
MOR (MPa)
\n
B (kg m−3]
\n
\n\n\n
\n
K
\n
6.4
\n
29.4
\n
2180
\n
1.9
\n
38.5
\n
2280
\n
\n
\n
CAC
\n
1.3
\n
58.9
\n
2360
\n
Melting of test samples
\n
\n\n
Table 4.
Physicomechanical properties of fired bodies K and CAC depending on firing temperature: Ev—water absorption, MOR—modulus of rupture, B—bulk density.
\n
\n
\n
4. Conclusions
\n
For sintering and melting of pure feldspar rocks, not just the total content of feldspar components is important, but also the ratio between potassium, sodium and calcium feldspars. At the appropriate ratio, low melting eutectics can be expected to rise, with a melting temperature substantially lower than the theoretical melting temperature of pure feldspars. The presence of calcium feldspar significantly reduces sintering ability and melting of feldspar rocks. Totally different results we can expect for the mixtures of feldspar rocks with the plastic part of whiteware raw materials mixture—kaolin. The reactions between feldspar rocks and kaolin (Al2O3, SiO2) during the sintering process are the cause of low melting eutectics, which accelerate sintering.
\n
Natural zeolite is very intensive fluxing agent for ceramic technology. Using zeolite we can reduce the sintering temperature of the body of about 100°C, compared with traditional ceramic fluxing agent—potassium‐sodium feldspar rock F‐KNa. The sintered body (with water absorption below 2%) based on zeolite has lower coefficient of linear thermal expansion. The presence of zeolite in raw materials mixture significantly changes mineralogical composition of fired whiteware body—mullite, anorthite and cristobalite are the main mineralogical phases instead of mullite and quartz, which are typical for a standard whiteware bodies made from raw material mixtures based on kaolin, quartz and feldspar. The limiting factor for the use of natural zeolite as a flux for whiteware is its coloring effect.
\n
Calcium aluminate cement CAC with high content of Al2O3 (70%) in the raw materials mixture for whiteware production is suitable alternative to kaolin—higher strength of green and fired body, more intensive whiteness of body after firing and lower coefficient of linear thermal expansion is possible to expect using CAC. The sintering activity of the whiteware body is accelerated when calcium aluminate cement is used as a binder instead of kaolin—the bodies can be fired at lower temperatures. Calcium aluminate cement significantly changes mineralogical composition of fired body—anorthite is the main mineralogical phase, mullite is typical phase for standard porcelain bodies made in the system of kaolin‐quartz‐feldspar rock.
\n
\n
Acknowledgments
\n
The results were achieved under the project no. LO1408 “AdMaS UP—Advanced Materials, Structures and Technologies”, supported by the Ministry of Education, Youth and Sports under the “National Sustainability Programme I” (chapter 2). The results were achieved under the project—the Czech Science Foundation, research project no. P104/13/23051S “Anorthite porcelain body on the basis of aluminous cement” (chapter 3).
\n
\n',keywords:"whitewares, feldspar rocks, zeolite, bone ash, kaolin, calcium aluminate cement, sintering temperature, water absorption, mineralogical composition",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/54832.pdf",chapterXML:"https://mts.intechopen.com/source/xml/54832.xml",downloadPdfUrl:"/chapter/pdf-download/54832",previewPdfUrl:"/chapter/pdf-preview/54832",totalDownloads:882,totalViews:247,totalCrossrefCites:0,totalDimensionsCites:2,hasAltmetrics:0,dateSubmitted:"October 12th 2016",dateReviewed:"February 23rd 2017",datePrePublished:null,datePublished:"February 7th 2018",dateFinished:null,readingETA:"0",abstract:"The sintering of whiteware (porcelain) body can be affected by using fluxing agents or binders. The chapter describes the sintering process of porcelain body in case of different fluxing agent (different feldspar rocks, bone ash, zeolite) and binder (kaolin vs. calcium aluminate cement) utilization in the porcelain raw material mixture. Sintering process is presented according to thermodilatometrical curves and sintering temperatures especially.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/54832",risUrl:"/chapter/ris/54832",book:{slug:"sintering-of-functional-materials"},signatures:"Radomir Sokolar",authors:[{id:"197992",title:"Associate Prof.",name:"Radomir",middleName:null,surname:"Sokolar",fullName:"Radomir Sokolar",slug:"radomir-sokolar",email:"sokolar.r@fce.vutbr.cz",position:null,institution:{name:"Palacký University, Olomouc",institutionURL:null,country:{name:"Czech Republic"}}}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Sintering of whiteware body depending on fluxing agent (feldspar rocks, bone ash, zeolite)",level:"1"},{id:"sec_3",title:"3. The effect of calcium aluminate cement as a binder for the sintering of whiteware bodies",level:"1"},{id:"sec_4",title:"4. Conclusions",level:"1"},{id:"sec_5",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'\nCarty WM, Senapati U. Porcelain—raw materials, processing, phase evolution, and mechanical behavior. Journal of American Ceramic Society. 1998;81:3-20\n'},{id:"B2",body:'\nRado P. An Introduction to the Technology of Pottery. Oxford: Pergamon Press; 1988\n'},{id:"B3",body:'\nStubna I, Slavikova J, Vozar L. Relationship between mechanical strength and Young’s modulus of porcelain. Industrial Ceramics, 2008;28(2):153-154\n'},{id:"B4",body:'\nBarth TFW. Feldspars. 1st ed. Bath: John Wiley & Sons; 1969\n'},{id:"B5",body:'\nNorton, FH. Fine Ceramics Technology and Applications. 1st ed. Malabar: R.E Krieger; 1970\n'},{id:"B6",body:'\nDas S. Kr, Dana K. Differences in densification behaviour of K‐ and Na‐feldspar‐containing porcelain bodies. Thermochimica Acta, 2003;406(1-2):199-206\n'},{id:"B7",body:'\nAlves HJ, Melchiades FG, Boschi AO. Effect of feldspar particle size on the porous microstructure and stain resistance of polished porcelain tiles. Journal of the European Ceramic Society, 2012;32(10):2095-2102\n'},{id:"B8",body:'\nKim K, Kim K, Hwang J. LCD waste glass as a substitute for feldspar in the porcelain sanitary ware production. Ceramics International. 2015;41(5):7097-7102\n'},{id:"B9",body:'\nTurkmen O, Kucuk A, Akpinar S. Effect of wollastonite addition on sintering of hard porcelain. Ceramics International. 2015;41(4):5505-5512\n'},{id:"B10",body:'\nSokolar R, Vodova L. Sintering behaviour of feldspar rocks. Research Inventy: International Journal of Engineering and Science. 2014;10:49-55\n'},{id:"B11",body:'\nSokolar, Vodova, L. The difference between traditional and bone porcelain body. Advanced Materials Research. 2015;1100:87-90\n'},{id:"B12",body:'\nIqbal Y, Messer PF, Lee WE. Microstructural evolution in bone China. British Ceramic Transactions. 2000;99:193-199\n'},{id:"B13",body:'\nIqbal Y, Messer PF, Lee WE. Non‐equilibrium microstructure of bone China. British Ceramic Transactions. 2000;99:110-116\n'},{id:"B14",body:'\nSt Pierre JPDS. Note on the System CaO‐Al2O3‐P2O5. Journal of the American Ceramic Society. 1956;39:147\n'},{id:"B15",body:'\nPoon CS, Lam L, Kou SC, Lin ZS. A study on the hydration rate of natural zeolite blended cement pastes. Construction and Building Materials. 1999;13(1999):427-432\n'},{id:"B16",body:'\nValipour M, Pargar F, Shekarchi M, Khani S. Comparing a natural pozzolan, zeolite, to metakaolin and silica fume in terms of their effect on the durability characteristics of concrete: a laboratory study. Construction and Building Materials. 2013;41(2013):879-888\n'},{id:"B17",body:'\nCanpolat F, Yilmaz K, Kose MM, Sumer M, Yurdusev MA. Use of zeolite, coal bottom ash and fly ash as replacement materials in cement production. Cement and Concrete Research. 2004;34(2004):731-735\n'},{id:"B18",body:'\nVejmelková E, Keppert M, Ondráček M, Černý R. Effect of natural zeolite on the properties of high performance concrete. Cement Wapno Beton. 2013;18(2013):150-159\n'},{id:"B19",body:'\nRanjbar MM, Madandoust R, Mousavi SY, Yosefi S. Effects of natural zeolite on the fresh and hardened properties of self‐compacted concrete. Construction and Building Materials. 2013;47(2013):806-813\n'},{id:"B20",body:'\nde Gennaro R, Cappelletti P, Cerri G, de Gennaro M, Dondi M, Guarini G, Langella A, Naimo D. Influence of zeolites on the sintering and technological properties of porcelain stoneware tiles. Journal of the European Ceramic Society. 2003;23(2003):2237-2245\n'},{id:"B21",body:'\nDemirkirana AS, Artirb R, Avcia E. Effect of natural zeolite addition on sintering kinetics of porcelain bodies. Journal of Materials Processing Technology. 2008;203(2008):465-470\n'},{id:"B22",body:'\nSukran Demirkiran A, Artir R, Avci E. Electrical resistivity of porcelain bodies with natural zeolite addition. Ceramics International. 2010;36(2010):917-921\n'},{id:"B23",body:'\nde Gennaro R, Dondi M, Cappelletti P, Cerri G, de’ Gennaro M, Guarini G, Langella A, Parlato L, Zanelli Ch. Zeolite–feldspar epiclastic rocks as flux in ceramic tile manufacturing. Microporous and Mesoporous Materials. 2007;105(2007):273-278\n'},{id:"B24",body:'\nSokolar R, Sveda M. The use of zeolite as fluxing agent for whitewares. Procedia Engineering. 2016;151:229-235\n'},{id:"B25",body:'\nTai W, Kimura K, Jinnai K. A new approach to anorthite porcelain bodies using nonplastic raw materials. Journal of the European Ceramic Society. 2002;22(2002):463\n'},{id:"B26",body:'\nTaskiran MU, Demirkol N, Capoglu A. A new porcelainised stoneware material based on anorthite. Journal of the European Ceramic Society. 2005;25(2005):293-300\n'},{id:"B27",body:'\nSokolar R, Vodova L. Sodium Hexametaphosphate as Deflocculation Agent for Calcium Aluminate Cements in Porcelain Body. Advanced Materials Research. 897:30-33\n'},{id:"B28",body:'\nEl Hafiane Y, Smith A, Bonnet JP, Tanouti B. Effect of a carboxylic acid on the rheological behavior of an aluminous cement paste and consequences on the properties of the hardened material. Journal of the European Ceramic Society. 2005;25(2005):1143\n'},{id:"B29",body:'\nEl Hafiane Y, Smith A, Chartier T, Abouliatim Y, Nibou L, Bonnet JP. Role of dispersant and humidity on the setting of millimetric films of aluminous cement prepared by tape casting. Journal of the European Ceramic Society. 2012;32(2012):2103\n'},{id:"B30",body:'\nLerdprom W, Chinnam RK, Jayaseelan DD, Lee WE. Porcelain production by direct sintering. Journal of the European Ceramic Society. 2016;36(16):4319-4325\n'},{id:"B31",body:'\nPotuzak M, Solvang M, Dingwell D. Temperature independent thermal expansivities of calcium aluminosilicates melts between 1150 and 1973 K in the system anorthite–wollostanite–gehlenite (An–Wo–Geh): a density model. Geochimica et Cosmochimica Acta. 2006;70(2006):3059-3074\n'},{id:"B32",body:'\nCamerucci MA, Urretavizcaya G, Castro MS, Cavalieri AL. Electrical properties and thermal expansion of cordierite and cordierite‐mullite materials. Journal of the European Ceramic Society. 2001;21(2001):2917-2923\n'},{id:"B33",body:'\nSokolar R, Vodova L. Whitevare bodies without Kaolin. Interceram. 2014;63(2014):19\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Radomir Sokolar",address:"sokolar.r@fce.vutbr.cz",affiliation:'
Faculty of Civil Engineering, Brno University of Technology, Brno, Czech Republic
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Mertens and Jacqueline Lecomte-Beckers",authors:[{id:"178364",title:"Dr.",name:"Anne",middleName:"Isabelle",surname:"Mertens",fullName:"Anne Mertens",slug:"anne-mertens"},{id:"179082",title:"Prof.",name:"Jacqueline",middleName:null,surname:"Lecomte-Beckers",fullName:"Jacqueline Lecomte-Beckers",slug:"jacqueline-lecomte-beckers"}]},{id:"50676",title:"Metal Powder Additive Manufacturing",slug:"metal-powder-additive-manufacturing",signatures:"Anatoliy Popovich and Vadim Sufiiarov",authors:[{id:"179005",title:"Ph.D.",name:"Vadim",middleName:null,surname:"Sufiiarov",fullName:"Vadim Sufiiarov",slug:"vadim-sufiiarov"},{id:"179594",title:"Prof.",name:"Anatoliy",middleName:null,surname:"Popovich",fullName:"Anatoliy Popovich",slug:"anatoliy-popovich"}]},{id:"50821",title:"Laser-Assisted 3D Printing of Functional Graded Structures from Polymer Covered Nanocomposites: A Self-Review",slug:"laser-assisted-3d-printing-of-functional-graded-structures-from-polymer-covered-nanocomposites-a-sel",signatures:"Igor Volyanskii and Igor V. Shishkovsky",authors:[{id:"178616",title:"Prof.",name:"Igor",middleName:"V.",surname:"Shishkovsky",fullName:"Igor Shishkovsky",slug:"igor-shishkovsky"}]}]}]},onlineFirst:{chapter:{type:"chapter",id:"70192",title:"Stability Constants of Metal Complexes in Solution",doi:"10.5772/intechopen.90183",slug:"stability-constants-of-metal-complexes-in-solution",body:'
1. Introduction
Stability constant of the formation of metal complexes is used to measure interaction strength of reagents. From this process, metal ion and ligand interaction formed the two types of metal complexes; one is supramolecular complexes known as host-guest complexes [1] and the other is anion-containing complexes. In the solution it provides and calculates the required information about the concentration of metal complexes.
Solubility, light, absorption conductance, partitioning behavior, conductance, and chemical reactivity are the complex characteristics which are different from their components. It is determined by various numerical and graphical methods which calculate the equilibrium constants. This is based on or related to a quantity, and this is called the complex formation function.
During the displacement process at the time of metal complex formation, some ions disappear and form a bonding between metal ions and ligands. It may be considered due to displacement of a proton from a ligand species or ions or molecules causing a drop in the pH values of the solution [2]. Irving and Rossotti developed a technique for the calculation of stability constant, and it is called potentiometric technique.
To determine the stability constant, Bjerrum has used a very simple method, and that is metal salt solubility method. For the studies of a larger different variety of polycarboxylic acid-, oxime-, phenol-containing metal complexes, Martel and Calvin used the potentiometric technique for calculating the stability constant. Those ligands [3, 4] which are uncharged are also examined, and their stability constant calculations are determined by the limitations inherent in the ligand solubility method. The limitations of the metal salt solubility method and the result of solubility methods are compared with this. M-L, MLM, and (M3) L are some types of examples of metal-ligand bonding. One thing is common, and that is these entire types metal complexes all have one ligand.
The solubility method can only usefully be applied to studies of such complexes, and it is best applied for ML; in such types of system, only ML is formed. Jacqueline Gonzalez and his co-worker propose to explore the coordination chemistry of calcium complexes. Jacqueline and et al. followed this technique for evaluate the as partial model of the manganese-calcium cluster and spectrophotometric studies of metal complexes, i.e., they were carried calcium(II)-1,4-butanediamine in acetonitrile and calcium(II)-1,2-ethylendiamine, calcium(II)-1,3-propanediamine by them.
Spectrophotometric programming of HypSpec and received data allows the determination of the formation of solubility constants. The logarithmic values, log β110 = 5.25 for calcium(II)-1,3-propanediamine, log β110 = 4.072 for calcium(II)-1,4-butanediamine, and log β110 = 4.69 for calcium(II)-1,2-ethylendiamine, are obtained for the formation constants [5]. The structure of Cimetidine and histamine H2-receptor is a chelating agent. Syed Ahmad Tirmizi has examined Ni(II) cimetidine complex spectrophotometrically and found an absorption peak maximum of 622 nm with respect to different temperatures.
Syed Ahmad Tirmizi have been used to taken 1:2 ratio of metal and cimetidine compound for the formation of metal complex and this satisfied by molar ratio data. The data, 1.40–2.4 × 108, was calculated using the continuous variation method and stability constant at room temperature, and by using the mole ratio method, this value at 40°C was 1.24–2.4 × 108. In the formation of lead(II) metal complexes with 1-(aminomethyl) cyclohexene, Thanavelan et al. found the formation of their binary and ternary complexes. Glycine, l-proline, l-alanine, l-isoleucine, l-valine, and l-leucine are α-amino acids, and these are important biologically [6]. These α-amino acids are also investigated by potentiometric technique at 32°C. The mixed ligands were also studied using these methods. 50% (v/v) DMSO-water medium used for the determination of acidity constants and their stability constants these type ligands. In a stepwise manner, the ternary complexes were synthesized.
Using the stability constant method, these ternary complexes were found out, and using the parameters such as Δ log K and log X, these ternary complex data were compared with binary complex. The potentiometric technique at room temperature (25°C) was used in the investigation of some binary complex formations by Abdelatty Mohamed Radalla. These binary complexes are formed with 3D transition metal ions like Cu2+, Ni2+, Co2+, and Zn2+ and gallic acid’s importance as a ligand and 0.10 mol dm−3 of NaNO3. Such types of aliphatic dicarboxylic acids are very important biologically. Many acid-base characters and the nature of using metal complexes have been investigated and discussed time to time by researchers [7].
The above acids (gallic and aliphatic dicarboxylic acid) were taken to determine the acidity constants. For the purpose of determining the stability constant, binary and ternary complexes were carried in the aqueous medium using the experimental conditions as stated above. The potentiometric pH-metric titration curves are inferred for the binary complexes and ternary complexes at different ratios, and formation of ternary metal complex formation was in a stepwise manner that provided an easy way to calculate stability constants for the formation of metal complexes.
The values of Δ log K, percentage of relative stabilization (% R. S.), and log X were evaluated and discussed. Now it provides the outline about the various complex species for the formation of different solvents, and using the concentration distribution, these complexes were evaluated and discussed. The conductivity measurements have ascertained for the mode of ternary chelating complexes.
A study by Kathrina and Pekar suggests that pH plays an important role in the formation of metal complexes. When epigallocatechin gallate and gallic acid combine with copper(II) to form metal complexes, the pH changes its speculation. We have been able to determine its pH in frozen and fluid state with the help of multifrequency EPR spectroscopy [8]. With the help of this spectroscopy, it is able to detect that each polyphenol exhibits the formation of three different mononuclear species. If the pH ranges 4–8 for di- or polymeric complex of Cu(II), then it conjectures such metal complexes. It is only at alkaline pH values.
The line width in fluid solutions by molecular motion exhibits an incomplete average of the parameters of anisotropy spin Hamilton. If the complexes are different, then their rotational correlation times for this also vary. The analysis of the LyCEP anisotropy of the fluid solution spectra is performed using the parameters determined by the simulation of the rigid boundary spectra. Its result suggests that pH increases its value by affecting its molecular mass. It is a polyphenol ligand complex with copper, showing the coordination of an increasing number of its molecules or increasing participation of polyphenol dimers used as ligands in the copper coordination region.
The study by Vishenkova and his co-worker [8] provides the investigation of electrochemical properties of triphenylmethane dyes using a voltammetric method with constant-current potential sweep. Malachite green (MG) and basic fuchsin (BF) have been chosen as representatives of the triphenylmethane dyes [9]. The electrochemical behavior of MG and BF on the surface of a mercury film electrode depending on pH, the nature of background electrolyte, and scan rate of potential sweep has been investigated.
Using a voltammetric method with a constant-current potential sweep examines the electrical properties of triphenylmethane dye. In order to find out the solution of MG and BF, certain registration conditions have been prescribed for it, which have proved to be quite useful. The reduction peak for the currents of MG and BF has demonstrated that it increases linearly with respect to their concentration as 9.0 × 10−5–7.0 × 10−3 mol/dm3 for MG and 6.0 × 10−5–8.0 × 10−3 mol/dm3 for BF and correlation coefficients of these values are 0.9987 for MG and 0.9961 for BF [10].
5.0 × 10−5 and 2.0 × 10−5 mol/dm3 are the values used as the detection limit of MG and BF, respectively. Stability constants are a very useful technique whose size is huge. Due to its usefulness, it has acquired an umbrella right in the fields of chemistry, biology, and medicine. No science subject is untouched by this. Stability constants of metal complexes are widely used in the various areas like pharmaceuticals as well as biological processes, separation techniques, analytical processes, etc. In the presented chapter, we have tried to explain this in detail by focusing our attention on the applications and solutions of stability of metal complexes in solution.
2. Stability constant of metal complexes
Stability or formation or binding constant is the type of equilibrium constant used for the formation of metal complexes in the solution. Acutely, stability constant is applicable to measure the strength of interactions between the ligands and metal ions that are involved in complex formation in the solution [11]. A generally these 1-4 equations are expressed as the following ways:
Metal+Ligand⇆Metal−LigandK1=MLMLE1
Metal+Ligands⇆Metal+Ligand2K2=ML2MLLE2
Metal+Ligand3⇆Metal+Ligand3K3=ML3ML2LE3
Thus
Metal+Ligandn−1+L⇆Metal+Ligand−nKn=MLnMLn−1LE4
K1, K2, K3, … Kn are the equilibrium constants and these are also called stepwise stability constants. The formation of the metal-ligand-n complex may also be expressed as equilibrium constants by the following steps:
Metal+Ligand→B1Metal−Ligand,β=MLMLE5
Metal+2Ligand→B2Metal−Ligand2,β2=ML2ML2E6
Thus Metal+nLigand→BnMetal−ligandLn,βn=MLnMLnE7
β1, β2, β3, … βn are the equilibrium constants, and these equilibrium constants are known as overall stability constants or overall formation. βn is called as the nth cumulative or overall formation constant [12]. Any metal complexes will be of greater stability if its stability constant has the higher value. Sometimes the 1/k values are alternative values of stability constant, and now this is called as instability constant. Log10K1, log10K2 … log10Kn, and log10βn are the ways that expressed the stepwise and cumulative stability constants.
3. Relationship or interaction between βn and K1, K2, K3, … Kn
The parameters K and β are related together, and these are expressed in the following example:
β3=ML3ML3E8
Now the numerator and denominator are multiplied together with the use of [metal-ligand] [metal-ligand2], and after the rearranging we get the following equation:
From the above relation, it is clear that the overall stability constant βn is equal to the product of the successive (i.e., stepwise) stability constants, K1, K2, K3,…Kn. This in other words means that the value of stability constants for a given complex is actually made up of a number of stepwise stability constants. The term stability is used without qualification to mean that the complex exists under a suitable condition and that it is possible to store the complex for an appreciable amount of time. The term stability is commonly used because coordination compounds are stable in one reagent but dissociate or dissolve in the presence of another regent. It is also possible that the term stability can be referred as an action of heat or light or compound. The stability of complex [13] is expressed qualitatively in terms of thermodynamic stability and kinetic stability.
3.1 Thermodynamic stability
In a chemical reaction, chemical equilibrium is a state in which the concentration of reactants and products does not change over time. Often this condition occurs when the speed of forward reaction becomes the same as the speed of reverse reaction. It is worth noting that the velocities of the forward and backward reaction are not zero at this stage but are equal.
If hydrogen and iodine are kept together in molecular proportions in a closed process vessel at high temperature (500°C), the following action begins:
H2+I2→2HIE12
In this activity, hydrogen iodide is formed by combining hydrogen and iodine, and the amount of hydrogen iodide increases with time. In contrast to this action, if the pure hydrogen iodide gas is heated to 500°C in the reaction, the compound is dissolved by reverse action, which causes hydrogen iodide to dissolve into hydrogen and iodine, and the ratio of these products increases over time. This is expressed in the following reaction:
2HI→H2+I2E13
For the formation of metal chelates, the thermodynamic technique provides a very significant information. Thermodynamics is a very useful technique in distinguishing between enthalpic effects and entropic effects. The bond strengths are totally effected by enthalpic effect, and this does not make any difference in the whole solution in order/disorder. Based on thermodynamics the chelate effect below can be best explained. The change of standard Gibbs free energy for equilibrium constant is response:
ΔG=−2.303RTlog10β.E14
Where:
R = gas constant
T = absolute temperature
At 25°C,
ΔG = (− 5.708 kJ mol−1) · log β.
The enthalpy term creates free energy, i.e.,
ΔG=ΔH–TΔSE15
For metal complexes, thermodynamic stability and kinetic stability are two interpretations of the stability constant in the solution. If reaction moves from reactants to products, it refers to a change in its energy as shown in the above equation. But for the reactivity, kinetic stability is responsible for this system, and this refers to ligand species [14].
Stable and unstable are thermodynamic terms, while labile and inert are kinetic terms. As a rule of thumb, those complexes which react completely within about 1 minute at 25°C are considered labile, and those complexes which take longer time than this to react are considered inert. [Ni(CN)4]2− is thermodynamically stable but kinetically inert because it rapidly exchanges ligands.
The metal complexes [Co(NH3)6]3+ and such types of other complexes are kinetically inert, but these are thermodynamically unstable. We may expect the complex to decompose in the presence of acid immediately because the complex is thermodynamically unstable. The rate is of the order of 1025 for the decomposition in acidic solution. Hence, it is thermodynamically unstable. However, nothing happens to the complex when it is kept in acidic solution for several days. While considering the stability of a complex, always the condition must be specified. Under what condition, the complex which is stable or unstable must be specified such as acidic and also basic condition, temperature, reactant, etc.
A complex may be stable with respect to a particular condition but with respect to another. In brief, a stable complex need not be inert and similarly, and an unstable complex need not be labile. It is the measure of extent of formation or transformation of complex under a given set of conditions at equilibrium [15].
Thermodynamic stability has an important role in determining the bond strength between metal ligands. Some complexes are stable, but as soon as they are introduced into aqueous solution, it is seen that these complexes have an effect on stability and fall apart. For an example, we take the [Co (SCN)4]2+ complex. The ion bond of this complex is very weak and breaks down quickly to form other compounds. But when [Fe(CN)6]3− is dissolved in water, it does not test Fe3+ by any sensitive reagent, which shows that this complex is more stable in aqueous solution. So it is indicated that thermodynamic stability deals with metal-ligand bond energy, stability constant, and other thermodynamic parameters.
This example also suggests that thermodynamic stability refers to the stability and instability of complexes. The measurement of the extent to which one type of species is converted to another species can be determined by thermodynamic stability until equilibrium is achieved. For example, tetracyanonickelate is a thermodynamically stable and kinetic labile complex. But the example of hexa-amine cobalt(III) cation is just the opposite:
CoNH363++6H3O+→CoH2O63++6NH4+E16
Thermodynamics is used to express the difference between stability and inertia. For the stable complex, large positive free energies have been obtained from ΔG0 reaction. The ΔH0, standard enthalpy change for this reaction, is related to the equilibrium constant, βn, by the well thermodynamic equation:
ΔG0=−RTlnβE17
ΔG0=ΔH0−TΔS0E18
For similar complexes of various ions of the same charge of a particular transition series and particular ligand, ΔS0 values would not differ substantially, and hence a change in ΔH0 value would be related to change in βn values. So the order of values of ΔH0 is also the order of the βn value.
3.2 Kinetic stability
Kinetic stability is referred to the rate of reaction between the metal ions and ligand proceeds at equilibrium or used for the formation of metal complexes. To take a decision for kinetic stability of any complexes, time is a factor which plays an important role for this. It deals between the rate of reaction and what is the mechanism of this metal complex reaction.
As we discuss above in thermodynamic stability, kinetic stability is referred for the complexes at which complex is inert or labile. The term “inert” was used by Tube for the thermally stable complex and for reactive complexes the term ‘labile’ used [16]. The naturally occurring chlorophyll is the example of polydentate ligand. This complex is extremely inert due to exchange of Mg2+ ion in the aqueous media.
4. Factors affecting the stability of complexes
The nature of central atom of metal complexes, dimension, its degree of oxidation, electronic structure of these complexes, and so many other properties of complexes are affected by the stability constant. Some of the following factors described are as follows.
4.1 Nature of central metal ion
In the coordination chemistry, metal complexes are formed by the interaction between metal ions and ligands. For these type of compounds, metal ions are the coordination center, and the ligand or complexing agents are oriented surrounding it. These metal ions mostly are the transition elements. For the determination of stability constant, some important characteristics of these metal complexes may be as given below.
4.2 Ionic size
Ligands are oriented around the central metal ions in the metal complexes. The sizes of these metal ions determine the number of ligand species that will be attached or ordinated (dative covalent) in the bond formation. If the sizes of these metal ions are increased, the stability of coordination compound defiantly decreased. Zn(II) metal ions are the central atoms in their complexes, and due to their lower size (0.74A°) as compared to Cd(II) size (0.97A°), metal ions are formed more stable.
Hence, Al3+ ion has the greatest nuclear charge, but its size is the smallest, and the ion N3− has the smallest nuclear charge, and its size is the largest [17]. Inert atoms like neon do not participate in the formation of the covalent or ionic compound, and these atoms are not included in isoelectronic series; hence, it is not easy to measure the radius of this type of atoms.
4.3 Ionic charge
The properties of stability depend on the size of the metal ion used in the complexes and the total charge thereon. If the size of these metal ions is small and the total charge is high, then their complexes will be more stable. That is, their ratio will depend on the charge/radius. This can be demonstrated through the following reaction:
Fe3++6CN−⇆FeCN63−logβ=31More StableE19
Fe2++6CN−⇆FeCN64−logβ=8.3Less StableE20
An ionic charge is the electric charge of an ion which is formed by the gain (negative charge) or loss (positive charge) of one or more electrons from an atom or group of atoms. If we talk about the stability of the coordination compounds, we find that the total charge of their central metal ions affects their stability, so when we change their charge, their stability in a range of constant can be determined by propagating of error [18]. If the charge of the central metal ion is high and the size is small, the stability of the compound is high:
Li+>Na+>K+>Rb+>Cs+E21
Th4+>Y3+>Ca2+>Na+andLa3+>Sr2+>K+E22
In general, the most stable coordination bonds can cause smaller and highly charged rations to form more stable coordination compounds.
4.4 Electronegativity
When an electron pair attracts a central ion toward itself, a strong stability complex is formed, and this is due to electron donation from ligand → metal ion. This donation process is increasing the bond stability of metal complexes exerted the polarizing effect on certain metal ions. Li+, Na+, Mg2+, Ca2+, Al3+, etc. are such type of metal cation which is not able to attract so strongly from a highly electronegative containing stable complexes, and these atoms are O, N, F, Au, Hg, Ag, Pd, Pt, and Pb. Such type of ligands that contains P, S, As, Br and I atom are formed stable complex because these accepts electron from M → π-bonding. Hg2+, Pb2+, Cd2+, and Bi3+ metal ions are also electronegative ions which form insoluble salts of metal sulfide which are insoluble in aqueous medium.
4.5 Temperature and pressure
Volatile ligands may be lost at higher temperature. This is exemplified by the loss of water by hydrates and ammonia:
CoNH36Cl3∆175−180°C→CoNH35ClCl2+NH3E23
The transformation of certain coordination compounds from one to another is shown as follows:
AgHgAgI4red45°C⇆Ag2HgI4yellowE24
4.6 Ligand nature
A ligand is an ion or small molecule that binds to a metal atom (in chemistry) or to a biomolecule (in biochemistry) to form a complex, such as the iron-cyanide coordination complex Prussian blue or the iron-containing blood-protein hemoglobin. The ligands are arranged in spectrochemical series which are based on the order of their field strength. It is not possible to form the entire series by studying complexes with a single metal ion; the series has been developed by overlapping different sequences obtained from spectroscopic studies [19]. The order of common ligands according to their increasing ligand field strength is
The above spectrochemical series help us to for determination of strength of ligands. The left last ligand is as weaker ligand. These weaker ligand cannot forcible binding the 3d electron and resultant outer octahedral complexes formed. It is as-Mn2+<Ni2+<Co2+<Fe2+<V2+<Fe3+<Cr3+<V3+<Co3+. For the given ligand, it is not possible to say about the exerted strong or weaker field on the central metal ion. The values of Δ are observed as:
Increasing the oxidation number the value of Δ increased.
Δ increases from top to bottom.
However, when we consider the metal ion, the following two useful trends are observed:
Δ increases with increasing oxidation number.
Δ increases down a group. For the determination of stability constant, the nature of the ligand plays an important role.
The following factors described the nature of ligands.
4.7 Size and charge
The size and charge are two factors that affect the production of metal complexes. The less charges and small sizes of ligands are more favorable for less stable bond formation with metal and ligand. But if this condition just opposite the product of metal and ligand will be a more stable compound. So, less nuclear charge and more size= less stable complex whereas if more nuclear charge and small in size= less stable complex. We take fluoride as an example because due to their smaller size than other halide and their highest electro negativity than the other halides formed more stable complexes. So, fluoride ion complexes are more stable than the other halides:
FeF2+logβ=6.0E26
FeCl2+logβ=1.3E27
As compared to S2− ion, O22− ions formed more stable complexes.
4.8 Basic character
It is suggested by Calvin and Wilson that the metal complexes will be more stable if the basic character or strength of ligands is higher. It means that the donating power of ligands to central metal ions is high [20].
It means that the donating power of ligands to central metal ions is high. In the case of complex formation of aliphatic diamines and aromatic diamines, the stable complex is formed by aliphatic diamines, while an unstable coordination complex is formed with aromatic diamines. So, from the above discussion, we find that the stability will be grater if the e-donation power is greater.
Thus it is clear that greater basic power of electron-donating species will form always a stable complex. NH3, CN−, and F− behaved as ligands and formed stable complexes; on the other hand, these are more basic in nature.
4.9 Ligand concentration
We know that if the concentration of coordination group is higher, these coordination compounds will exist in the water as solution. It is noted that greater coordinating tendency show the water molecules than the coordinating group which is originally present. SCN− (thiocynate) ions are present in higher concentration; with the Co2+ metal ion, it formed a blue-colored complex which is stable in state, but on dilution of water medium, a pink color is generated in place of blue, or blue color complex is destroyed by [Co(H2O)6]2+, and now if we added further SCN−, the pink color will not appear:
CoSCN42−+H2O⇆CoH2O62++4SCN−BluePinkE28
Now it is clear that H2O and SCN− are in competition for the formation of Co(II) metal-containing complex compound. In the case of tetra-amine cupric sulfate metal complex, ammonia acts as a donor atom or ligand. If the concentration of NH3 is lower in the reaction, copper hydroxide is formed but at higher concentration formed tetra-amine cupric sulfate as in the following reaction:
CuSO4+NH4OH→CuOH2Small quantity of ligandE29
CuSO4+NH4OH→CuOH2CuNH42SO4.H2OHigh concentration of ligandE30
4.10 Chelating effect
For a metal ion, chelating ligand is enhanced and affinity it and this is known as chelate effect and compared it with non-chelating and monodentate ligand or the multidentate ligand is acts as chelating agent. Ethylenediamine is a simple chelating agent (Figure 1).
Figure 1.
Structure of ethylenediamine.
Due to the bidentate nature of ethylenediamine, it forms two bonds with metal ion or central atom. Water forms a complex with Ni(II) metal ion, but due to its monodentate nature, it is not a chelating ligand (Figures 2 and 3).
Figure 2.
Structure of chelating configuration of ethylenediamine ligand.
Figure 3.
Structure of chelate with three ethylenediamine ligands.
The dentate cheater of ligand provides bonding strength to the metal ion or central atom, and as the number of dentate increased, the tightness also increased. This phenomenon is known as chelating effect, whereas the formation of metal complexes with these chelating ligands is called chelation:
Metal+2Ligand↔MetalLigand2K=ML2ML2E31
Metal+Ligand–Ligand↔MetalLigand−LigandE32
or
E33
Some factors are of much importance for chelation as follows.
4.11 Ring size
The sizes of the chelating ring are increased as well as the stability of metal complex decreased. According to Schwarzenbach, connecting bridges form the chelating rings. The elongated ring predominates when long bridges connect to the ligand to form a long ring. It is usually observed that an increased a chelate ring size leads to a decrease in complex stability.
He interpreted this statement. The entropy of complex will be change if the size of chelating ring is increased, i.e., second donor atom is allowed by the chelating ring. As the size of chelating ring increased, the stability should be increased with entropy effect. Four-membered ring compounds are unstable, whereas five-membered are more stable. So the chelating ring increased its size and the stability of the formed metal complexes.
4.12 Number of rings
The number of chelating rings also decides the stability of complexes. Non-chelating metal compounds are less stable than chelating compounds. These numbers increase the thermodynamic volume, and this is also known as an entropy term. In recent years ligands capable of occupying as many as six coordination positions on a single metal ion have been described. The studies on the formation constants of coordination compounds with these ligands have been reported. The numbers of ligand or chelating agents are affecting the stability of metal complexes so as these numbers go up and down, the stability will also vary with it.
For the Ni(II) complexes with ethylenediamine as chelating agent, its log K1 value is 7.9 and if chelating agents are trine and penten, then the log K1 values are 7.9 and 19.3, respectively. If the metal ion change Zn is used in place of Ni (II), then the values of log K1 for ethylenediamine, trine, and penten are 6.0, 12.1, and 16.2, respectively. The log βMY values of metal ions are given in Table 1.
Metal ion
log βMY (25°C, I = 0.1 M)
Ca2+
11.2
Cu2+
19.8
Fe3+
24.9
Table 1.
Metal ion vs. log βMY values.
Ni(NH3)62+ is an octahedral metal complex, and at 25 °C its log β6 value is 8.3, but Ni(ethylenediamine)32+ complex is also octahedral in geometry, with 18.4 as the value of log β6. The calculated stability value of Ni(ethylenediamine)32+ 1010 times is more stable because three rings are formed as chelating rings by ethylenediamine as compared to no such ring is formed. Ethylenediaminetetraacetate (EDTA) is a hexadentate ligand that usually formed stable metal complexes due to its chelating power.
4.13 Steric effect
A special effect in molecules is when the atoms occupy space. This is called steric effect. Energy is needed to bring these atoms closer to each other. These electrons run away from near atoms. There can be many ways of generating it. We know the repulsion between valence electrons as the steric effect which increases the energy of the current system [21]. Favorable or unfavorable any response is created.
For example, if the static effect is greater than that of a product in a metal complex formation process, then the static increase would favor this reaction. But if the case is opposite, the skepticism will be toward retardation.
This effect will mainly depend on the conformational states, and the minimum steric interaction theory can also be considered. The effect of secondary steric is seen on receptor binding produced by an alternative such as:
Reduced access to a critical group.
Stick barrier.
Electronic resonance substitution bond by repulsion.
Population of a conformer changes due to active shielding effect.
4.14 Macrocyclic effect
The macrocyclic effect is exactly like the image of the chelate effect. It means the principle of both is the same. But the macrocyclic effect suggests cyclic deformation of the ligand. Macrocyclic ligands are more tainted than chelating agents. Rather, their compounds are more stable due to their cyclically constrained constriction. It requires some entropy in the body to react with the metal ion. For example, for a tetradentate cyclic ligand, we can use heme-B which forms a metal complex using Fe+2 ions in biological systems (Figure 4).
Figure 4.
Structure of hemoglobin is the biological complex compound which contains Fe(II) metal ion.
The n-dentate chelating agents play an important role for the formation of more stable metal complexes as compared to n-unidentate ligands. But the n-dentate macrocyclic ligand gives more stable environment in the metal complexes as compared to open-chain ligands. This change is very favorable for entropy (ΔS) and enthalpy (ΔH) change.
5. Determination of stability constants of complexes in solution
There are so many parameters to determination of formation constants or stability constant in solution for all types of chelating agents. These numerous parameters or techniques are refractive index, conductance, temperature, distribution coefficients, refractive index, nuclear magnetic resonance volume changes, and optical activity.
5.1 Methods based on study of heterogeneous equilibrium
5.1.1 Solubility methods
Solubility products are helpful and used for the insoluble salt that metal ions formed and complexes which are also formed by metal ions and are more soluble. The formation constant is observed in presence of donor atoms by measuring increased solubility.
5.1.2 Distribution method
To determine the solubility constant, it involves the distribution of the ligands or any complex species; metal ions are present in two immiscible solvents like water and carbon tetrachloride, benzene, etc.
5.1.3 Ion exchange method
In this method metal ions or ligands are present in solution and on exchanger. A solid polymers containing with positive and negative ions are ion exchange resins. These are insoluble in nature. This technique is helpful to determine the metal ions in resin phase, liquid phase, or even in radioactive metal. This method is also helpful to determine the polarizing effect of metal ions on the stability of ligands like Cu(II) and Zn(II) with amino acid complex formation.
5.1.4 Electrometric techniques
At the equilibrium free metal and ions are present in the solution, and using the different electrometric techniques as described determines its stability constant.
5.1.5 Potentiometric methods
This method is based upon the titration method or follows its principle. A stranded acid-base solution used as titrate and which is titrated, it may be strong base or strong acid follows as potentiometrically. The concentration of solution using 103− M does not decomposed during the reaction process, and this method is useful for protonated and nonprotonated ligands.
5.1.6 Polarographic method
This is the graphic method used to determine the stability constant in producing metal complex formation by plotting a polarograph between the absences of substances and the presence of substances. During the complex formation, the presence of metal ions produced a shift in the half-wave potential in the solution.
5.2 Other methods
5.2.1 Rate method
If a complex is relatively slow to form and also decomposes at measurable rate, it is possible, in favorable situations, to determine the equilibrium constant.
5.2.2 Freezing technique
This involves the study of the equilibrium constant of slow complex formation reactions. The use of tracer technique is extremely useful for determining the concentrations of dissociation products of the coordination compound.
5.2.3 Biological method
This method is based on the study of the effect of an equilibrium concentration of some ions on the function at a definite organ of a living organism. The equilibrium concentration of the ion studied may be determined by the action of this organ in systems with complex formation.
5.2.4 Spectrophotometric method
The solution of 25 ml is adopted by preparing at the 1.0 × 10−5 M ligand or 1.0 × 10−5 M concentration and 1.0 × 10−5 M for the metal ion:
The solutions containing the metal ions were considered both at a pH sufficiently high to give almost complete complexation and at a pH value selected in order to obtain an equilibrium system of ligand and complexes.
In order to avoid modification of the spectral behavior of the ligand due to pH variations, it has been verified that the range of pH considered in all cases does not affect absorbance values. Use the collected pH values adopted for the determinations as well as selected wavelengths. The ionic strengths calculated from the composition of solutions allowed activity coefficient corrections. Absorbance values were determined at wavelengths in the range 430–700 nm, every 2 nm.
5.2.5 Bjerrum’s method
For a successive metal complex formation, use this method. If ligand is protonate and the produced complex has maximum number of donate atoms of ligands, a selective light is absorbed by this complex, while for determination of stability constant, it is just known about the composition of formed species.
Bjerrum (1941) used the method stepwise addition of the ligands to coordination sphere for the formation of complex. So, complex metal–ligand-n forms as the following steps [22]. The equilibrium constants, K1, K2, K3, … Kn are called stepwise stability constants. The formation of the complex metal-ligandn may also be expressed by the following steps and equilibrium constants.
Where:
M = central metal cation
L = monodentate ligand
N = maximum coordination number for the metal ion M for the ligand
If a complex ion is slow to reach equilibrium, it is often possible to apply the method of isotopic dilution to determine the equilibrium concentration of one or more of the species. Most often radioactive isotopes are used.
5.2.7 Conductance measurement method
This method was extensively used by Werner and others to study metal complexes. In the case of a series of complexes of Co(III) and Pt(IV), Werner assigned the correct formulae on the basis of their molar conductance values measured in freshly prepared dilute solutions. In some cases, the conductance of the solution increased with time due to a chemical change, e.g.,
CoNH34Br2++2H2OCoNH34H2O23++2Br−E38
6. Conclusion
It is concluded that the information presented is very important to determine the stability constant of the ligand metal complexes. Some methods like spectrophotometric method, Bjerrum’s method, distribution method, ion exchange method, electrometric techniques, and potentiometric method have a huge contribution in quantitative analysis by easily finding the stability constants of metal complexes in aqueous solutions.
Acknowledgments
All the authors thank the Library of University of Delhi for reference books, journals, etc. which helped us a lot in reviewing the chapter.
\n',keywords:"thermodynamic stability, kinetic stability, chelate effect, distribution method, ion exchange method, Bjerrum’s method",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/70192.pdf",chapterXML:"https://mts.intechopen.com/source/xml/70192.xml",downloadPdfUrl:"/chapter/pdf-download/70192",previewPdfUrl:"/chapter/pdf-preview/70192",totalDownloads:1220,totalViews:0,totalCrossrefCites:0,dateSubmitted:"April 10th 2019",dateReviewed:"October 16th 2019",datePrePublished:"November 25th 2019",datePublished:null,dateFinished:null,readingETA:"0",abstract:"In the formation of metal complexes in an aqueous medium, equilibrium constant or stability constant is used to determine the strength of interaction between reagents that make the final product after the formation of bonds. In general stability means that a complex may be stored for a long time under suitable conditions or this compound may be existing under suitable conditions. Regarding how much is the concentration of complexes in solution, stability constant provides this information via calculations. These calculations are very much important in many areas of science like chemistry, biology, and medicine. During the complex formation in aqueous medium, two types of stabilities are considered: one is the thermodynamic stability, and the other is kinetic stability. Stability of metal complexes may be affected by various factors like nature of central metal ion and ligand, chelating effect, etc., and some parameters like distribution coefficients, conductance, refractive index, etc. are useful for the determination of stability constants. Various modern techniques are used to determine the stability constant of simple as well as mixed ligand compounds.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/70192",risUrl:"/chapter/ris/70192",signatures:"Jagvir Singh, Abhay Nanda Srivastav, Netrapal Singh and Anuradha Singh",book:{id:"9190",title:"Stability and Applications of Coordination Compounds",subtitle:null,fullTitle:"Stability and Applications of Coordination Compounds",slug:"stability-and-applications-of-coordination-compounds",publishedDate:"July 8th 2020",bookSignature:"Abhay Nanda Srivastva",coverURL:"https://cdn.intechopen.com/books/images_new/9190.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"293623",title:"Dr.",name:"Abhay Nanda",middleName:"Nanda",surname:"Srivastva",slug:"abhay-nanda-srivastva",fullName:"Abhay Nanda Srivastva"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:null,sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Stability constant of metal complexes",level:"1"},{id:"sec_3",title:"3. Relationship or interaction between βn and K1, K2, K3, … Kn",level:"1"},{id:"sec_3_2",title:"3.1 Thermodynamic stability",level:"2"},{id:"sec_4_2",title:"3.2 Kinetic stability",level:"2"},{id:"sec_6",title:"4. Factors affecting the stability of complexes",level:"1"},{id:"sec_6_2",title:"4.1 Nature of central metal ion",level:"2"},{id:"sec_7_2",title:"4.2 Ionic size",level:"2"},{id:"sec_8_2",title:"4.3 Ionic charge",level:"2"},{id:"sec_9_2",title:"4.4 Electronegativity",level:"2"},{id:"sec_10_2",title:"4.5 Temperature and pressure",level:"2"},{id:"sec_11_2",title:"4.6 Ligand nature",level:"2"},{id:"sec_12_2",title:"4.7 Size and charge",level:"2"},{id:"sec_13_2",title:"4.8 Basic character",level:"2"},{id:"sec_14_2",title:"4.9 Ligand concentration",level:"2"},{id:"sec_15_2",title:"4.10 Chelating effect",level:"2"},{id:"sec_16_2",title:"4.11 Ring size",level:"2"},{id:"sec_17_2",title:"4.12 Number of rings",level:"2"},{id:"sec_18_2",title:"4.13 Steric effect",level:"2"},{id:"sec_19_2",title:"4.14 Macrocyclic effect",level:"2"},{id:"sec_21",title:"5. Determination of stability constants of complexes in solution",level:"1"},{id:"sec_21_2",title:"5.1 Methods based on study of heterogeneous equilibrium",level:"2"},{id:"sec_21_3",title:"5.1.1 Solubility methods",level:"3"},{id:"sec_22_3",title:"5.1.2 Distribution method",level:"3"},{id:"sec_23_3",title:"5.1.3 Ion exchange method",level:"3"},{id:"sec_24_3",title:"5.1.4 Electrometric techniques",level:"3"},{id:"sec_25_3",title:"5.1.5 Potentiometric methods",level:"3"},{id:"sec_26_3",title:"5.1.6 Polarographic method",level:"3"},{id:"sec_28_2",title:"5.2 Other methods",level:"2"},{id:"sec_28_3",title:"5.2.1 Rate method",level:"3"},{id:"sec_29_3",title:"5.2.2 Freezing technique",level:"3"},{id:"sec_30_3",title:"5.2.3 Biological method",level:"3"},{id:"sec_31_3",title:"5.2.4 Spectrophotometric method",level:"3"},{id:"sec_32_3",title:"5.2.5 Bjerrum’s method",level:"3"},{id:"sec_33_3",title:"5.2.6 Isotopic dilution method",level:"3"},{id:"sec_34_3",title:"5.2.7 Conductance measurement method",level:"3"},{id:"sec_37",title:"6. Conclusion",level:"1"},{id:"sec_38",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'Rossotti HS. Limitations of the ligand solubility method for studying complex formation. Journal of Inorganic and Nuclear Chemistry. Apr 1960;13(1-2):18-21'},{id:"B2",body:'Jacqueline GG, Monica NL, Varinia LR, Juan ARV, Jose JN, Segoviano G. Spectrophotometric determination of the formation constants of Calcium(II) complexes with 1,2-ethylenediamine, 1,3-propanediamine and 1,4-butanediamine in acetonitrile. Journal of Green Energy & Environment (KeAi). 2017;1:51-57'},{id:"B3",body:'Syed AT, Feroza HW, Muhammad HSW, Saadia S, Allah NM, Allah BG. Spectrophotometric study of stability constants of cimetidine–Ni(II) complex at different temperatures. Arabian Journal of Chemistry. 2012;2:309-314'},{id:"B4",body:'Thanavelan R, Ramalingam G, Manikandan G, Thanikachalam V. Stability constants of mixed ligand complexes of lead(II) with 1-(aminomethyl) cyclohexane acetic acid and α-amino acids. Journal of Saudi Chemical Society. 2014;18(3):227-233'},{id:"B5",body:'Abdelatty MR. Potentiometric studies on ternary complexes involving some divalent transition metal ions, gallic acid and biologically abundant aliphatic dicarboxylic acids in aqueous solutions, Beni-Suef University. Journal of Basic and Applied Sciences. 2015;4(2):174-182'},{id:"B6",body:'Katharina FP, Maria CB, Riccardo B, Bernard AG. Influence of pH on the speciation of copper(II) in reactions with the green tea polyphenols, epigallocatechin gallate and gallic acid. Journal of Inorganic Chemistry. 2012;112:10-16'},{id:"B7",body:'Vishenkova DA, Korotkova EI, Sokolova VA, Ratochvil BK. Electrochemical determination of some triphenylmethane dyes by means of voltammetry. Procedia Chemistry. 2015;15:109-114'},{id:"B8",body:'Lorenzo T, Zsolt B, Luca G, Attila F, Adrienn VMB. Thermodynamic stability, kinetic inertness and relaxometric properties of monoamide derivatives of lanthanide(III) DOTA complexes. Dalton Transactions. 2015;44:5467-5478'},{id:"B9",body:'Nagypal I. Chemistry of complex equilibria. Horwood. 1990;85312:143-145'},{id:"B10",body:'Dyrssen D, Ingri N, Sillen LG. Pit-mapping—A general approach to computer refinement of stability constants. Acta Chemica Scandinavica. 1961;15:694-696'},{id:"B11",body:'Ingri N, Sillen LG. High-speed computers as a supplement to graphical methods. Arkivor Kemi. 1964;23:97-121'},{id:"B12",body:'Sayce IG. Computer calculations of equilibrium constants of species present in mixtures of metal ions and complexing reagents. Talanta. 1968;15(12):1397-1421'},{id:"B13",body:'Sabatini A, Vacca A, Gans P. MINIQUAD—A general computer program for the computation of stability constants. Talanta. 1974;21(1):53-77'},{id:"B14",body:'Pearson RG. Chemical Hardness: Applications from Molecules to Solids. Manhattan, New York City: Springer-VCH; 2005. p. 210. ISBN: 978-3-527-60617-7'},{id:"B15",body:'Drago RS, Wong N, Bilgrien C, Vogel C. E and C parameters from Hammett substituent constants and use of E and C to understand cobalt-carbon bond energies. Inorganic Chemistry. 1987;26(1):9-14'},{id:"B16",body:'Vacca A, Nativi C, Cacciarini M, Pergoli R, Roelens S. A new tripodal receptor for molecular recognition of monosaccharides. A paradigm for assessing glycoside binding affinities and selectivity by 1H NMR spectroscopy. Journal of the American Chemical Society. 2004;126(50):16456-16465'},{id:"B17",body:'Marcotte N, Taglietti A. Transition-metal-based chemo sensing ensembles: ATP sensing in physiological conditions. Supramolecular Chemistry. 2003;15(7):617-717'},{id:"B18",body:'Boiocchi M, Bonizzoni M, Fabbrizzi L, Piovani G, Taglietti A. A di-metallic cage with a long ellipsoidal cavity for the fluorescent detection of dicarboxylate anions in water. Angewandte Chemie, International Edition. 2004;43(29):3847-3852'},{id:"B19",body:'Gampp M, Maeder M, Mayer CJ, Zuberbuhler AD. Calculation of equilibrium constants from multiwavelength spectroscopic data-I: Mathematical considerations. Talanta. 1985;32'},{id:"B20",body:'Frassineti C, Alderighi L, Gans P, Sabatini A, Vacca A, Ghelli S. Determination of protonation constants of some fluorinated polyamines by means of 13C NMR data processed by the new computer program Hyp-NMR 2000. Protonation sequence in polyamines. Analytical and Bioanalytical Chemistry. 2003;376(7):1041-1052'},{id:"B21",body:'Jiaxin Z, Guoyu T, Peng S. Understanding thermodynamic and kinetic contributions in expanding the stability window of aqueous electrolytes. 2018;4(12):2872-2882'},{id:"B22",body:'Gans P, Sabatini A, Vacca A. Investigation of equilibria in solution. Determination of equilibrium constants with the HYPERQUAD suite of programs. Talanta. 1996;43(10):1739-1753'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Jagvir Singh",address:"singhjagvir0143@gmail.com",affiliation:'
Department of Chemistry, ARSD College, University of Delhi, India
Department of Zoology, Raghuveer Singh Govt Degree College, India
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The Open Access model is applied to all of our publications and is designed to eliminate subscriptions and pay-per-view fees. This approach ensures free, immediate access to full text versions of your research.
As a gold Open Access publisher, an Open Access Publishing Fee is payable on acceptance following peer review of the manuscript. In return, we provide high quality publishing services and exclusive benefits for all contributors. IntechOpen is the trusted publishing partner of over 118,000 international scientists and researchers.
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Services included are:
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XML Typesetting and pagination - web (PDF, HTML) and print files preparation
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Permanent and unrestricted online access to your work
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Exceeds 20 pages (for chapters in Edited Volumes), an additional fee of 40 GBP per page will be required
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If a manuscript requires Heavy Editing or Language Polishing, this will incur additional fees.
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Your Author Service Manager will inform you of any items not covered by the OAPF and provide exact information regarding those additional costs before proceeding.
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Open Access Funding
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For Authors who are still unable to obtain funding from their institutions or research funding bodies for individual projects, IntechOpen does offer the possibility of applying for a Waiver to offset some or all processing feed. Details regarding our Waiver Policy can be found here.
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Added Value of Publishing with IntechOpen
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Indexing and listing across major repositories, see details ...
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Dissemination and Promotion
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Proven world leader in Open Access book publishing with over 10 years experience
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+108,170 citations in Web of Science databases
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Currently strongest OA platform with over 130 million downloads
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OAPF Publishing Options
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1,400 GBP Chapter - Edited Volume
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4,000 GBP Compacts Monograph - Short Form
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*These prices do not include Value-Added Tax (VAT). Residents of European Union countries need to add VAT based on the specific rate in their country of residence. Institutions and companies registered as VAT taxable entities in their own EU member state will not pay VAT as long as provision of the VAT registration number is made during the application process. This is made possible by the EU reverse charge method.
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Services included are:
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An online manuscript tracking system to facilitate your work
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Personal contact and support throughout the publishing process from your dedicated Author Service Manager
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Assurance that your manuscript meets the highest publishing standards
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English language copyediting and proofreading, including the correction of grammatical, spelling, and other common errors
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XML Typesetting and pagination - web (PDF, HTML) and print files preparation
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Permanent and unrestricted online access to your work
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Exceeds 20 pages (for chapters in Edited Volumes), an additional fee of 40 GBP per page will be required
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If a manuscript requires Heavy Editing or Language Polishing, this will incur additional fees.
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Your Author Service Manager will inform you of any items not covered by the OAPF and provide exact information regarding those additional costs before proceeding.
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Open Access Funding
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To explore funding opportunities and learn more about how you can finance your IntechOpen publication, go to our Open Access Funding page. IntechOpen offers expert assistance to all of its Authors. We can support you in approaching funding bodies and institutions in relation to publishing fees by providing information about compliance with the Open Access policies of your funder or institution. We can also assist with communicating the benefits of Open Access in order to support and strengthen your funding request and provide personal guidance through your application process. You can contact us at oapf@intechopen.com for further details or assistance.
\n\n
For Authors who are still unable to obtain funding from their institutions or research funding bodies for individual projects, IntechOpen does offer the possibility of applying for a Waiver to offset some or all processing feed. Details regarding our Waiver Policy can be found here.
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Added Value of Publishing with IntechOpen
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Indexing and listing across major repositories, see details ...
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Long-term archiving
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Visibility on the world's strongest OA platform
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Live Performance Metrics to track readership and the impact of your chapter
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Dissemination and Promotion
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Benefits of Publishing with IntechOpen
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Proven world leader in Open Access book publishing with over 10 years experience
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Most competitive prices in the market
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Optimized processes, enabling publication between 8 and 12 months
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Personal support during every step of the publication process
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+108,170 citations in Web of Science databases
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Currently strongest OA platform with over 130 million downloads
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