After the equilibrium point we know the equilibrium concentrations of CdY2- and EDTA. As we add EDTA, however, the reaction, $\mathrm{Cu(NH_3)_4^{2+}}(aq)+\textrm Y^{4-}(aq)\rightarrow\textrm{CuY}^{2-}(aq)+4\mathrm{NH_3}(aq)$, decreases the concentration of Cu(NH3)42+ and decreases the absorbance until we reach the equivalence point. The amount of EDTA reacting with Cu is, $\mathrm{\dfrac{0.06316\;mol\;Cu^{2+}}{L}\times0.00621\;L\;Cu^{2+}\times\dfrac{1\;mol\;EDTA}{mol\;Cu^{2+}}=3.92\times10^{-4}\;mol\;EDTA}$. The description here is based on Method 2340C as published in Standard Methods for the Examination of Water and Wastewater, 20th Ed., American Public Health Association: Washington, D. C., 1998. Of the cations contributing to hardness, Mg2+ forms the weakest complex with EDTA and is the last cation to be titrated. Report the sample’s hardness as mg CaCO3/L. Cyanide is determined at concentrations greater than 1 mg/L by making the sample alkaline with NaOH and titrating with a standard solution of AgNO3, forming the soluble Ag(CN)2– complex. After filtering and rinsing the precipitate, it is dissolved in 25.00 mL of 0.02011 M EDTA. The fully protonated form of EDTA, H6Y2+, is a hexaprotic weak acid with successive pKa values of. A 50.00-mL aliquot of the sample, treated with pyrophosphate to mask the Fe and Cr, required 26.14 mL of 0.05831 M EDTA to reach the murexide end point. where Kf´ is a pH-dependent conditional formation constant. Figure 9.35 Spectrophotometric titration curve for the complexation titration of a mixture of two analytes. What problems might you expect at a higher pH or a lower pH? Since EDTA is insoluble in water, the disodium salt of EDTA is taken for this experiment. Report the molar concentration of EDTA in the titrant. When the titration is complete, raising the pH to 9 allows for the titration of Ca2+. Because of calmagite’s acid–base properties, the range of pMg values over which the indicator changes color is pH–dependent (Figure 9.30). leaving 4.58×10–4 mol of EDTA to react with Cr. A 0.4071-g sample of CaCO3 was transferred to a 500-mL volumetric flask, dissolved using a minimum of 6 M HCl, and diluted to volume. Complexometric Titrations. Note that the titration curve’s y-axis is not the actual absorbance, A, but a corrected absorbance, Acorr, $A_\textrm{corr}=A\times\dfrac{V_\textrm{EDTA}+V_\textrm{Cu}}{V_\textrm{Cu}}$. The stoichiometry between EDTA and each metal ion is 1:1. The actual number of coordination sites depends on the size of the metal ion, however, all metal–EDTA complexes have a 1:1 stoichiometry. Suppose we need to analyze a mixture of Ni2+ and Ca2+. The LibreTexts libraries are Powered by MindTouch® and are supported by the Department of Education Open Textbook Pilot Project, the UC Davis Office of the Provost, the UC Davis Library, the California State University Affordable Learning Solutions Program, and Merlot. Now that we know something about EDTA’s chemical properties, we are ready to evaluate its usefulness as a titrant. See the text for additional details. Figure 9.29a shows the result of the first step in our sketch. Record the titration volumes. In the section we review the general application of complexation titrimetry with an emphasis on applications from the analysis of water and wastewater. As we add EDTA it reacts first with free metal ions, and then displaces the indicator from MInn–. A similar calculation should convince you that pCd = logKf´ when the volume of EDTA is 2×Veq. For a titration using EDTA, the stoichiometry is always 1:1. A late end point and a positive determinate error are possible if we use a pH of 11. The molarity of EDTA in the titrant is, $\mathrm{\dfrac{4.068\times10^{-4}\;mol\;EDTA}{0.04263\;L\;EDTA} = 9.543\times10^{-3}\;M\;EDTA}$. Add 1–2 drops of indicator and titrate with a standard solution of EDTA until the red-to-blue end point is reached (Figure 9.32). A comparison of our sketch to the exact titration curve (Figure 9.29f) shows that they are in close agreement. Titration | Unless otherwise noted, LibreTexts content is licensed by CC BY-NC-SA 3.0. The end point is determined by plotting the P ... to the suitable buffer solution and appropriate indicator solution and the resulting solution is titrated with the EDTA solution. Other metal–ligand complexes, such as CdI42–, are not analytically useful because they form a series of metal–ligand complexes (CdI+, CdI2(aq), CdI3– and CdI42–) that produce a sequence of poorly defined end points. The solid lines are equivalent to a step on a conventional ladder diagram, indicating conditions where two (or three) species are equal in concentration. Most indicators for complexation titrations are organic dyes—known as metallochromic indicators—that form stable complexes with metal ions. It is also not good for fish tanks. EDTA is a versatile titrant that can be used to analyze virtually all metal ions. Cations with higher charges (like Bi3+, Fe3+) have much larger stability constants, so they can be titrated at low pH, in the presence of divalent cations (like Ca2+, Mg2+) which will not interfere in this conditions. C_\textrm{EDTA}&=\dfrac{M_\textrm{EDTA}V_\textrm{EDTA}-M_\textrm{Cd}V_\textrm{Cd}}{V_\textrm{Cd}+V_\textrm{EDTA}}\\ Titrating with EDTA using murexide or Eriochrome Blue Black R as the indicator gives the concentration of Ca2+. Acid-Base | 2. Standardization is accomplished by titrating against a solution prepared from primary standard grade NaCl. Practical analytical applications of complexation titrimetry were slow to develop because many metals and ligands form a series of metal–ligand complexes. Recall that an acid–base titration curve for a diprotic weak acid has a single end point if its two Ka values are not sufficiently different. After adding calmagite as an indicator, the solution was titrated with the EDTA, requiring 42.63 mL to reach the end point. At a pH of 3 the CaY2– complex is too weak to successfully titrate. The first four values are for the carboxylic acid protons and the last two values are for the ammonium protons. To prevent an interference the pH is adjusted to 12–13, precipitating Mg2+ as Mg(OH)2. Complexometric titration » EDTA. Explore more on EDTA. &=\dfrac{\textrm{(0.0100 M)(30.0 mL)} - (5.00\times10^{-3}\textrm{ M})(\textrm{50.0 mL})}{\textrm{50.0 mL + 30.0 mL}}\\ Figure 9.27 shows a ladder diagram for EDTA. From Table 9.10 and Table 9.11 we find that αY4– is 0.35 at a pH of 10, and that αCd2+ is 0.0881 when the concentration of NH3 is 0.0100 M. Using these values, the conditional formation constant is, $K_\textrm f''=K_\textrm f \times \alpha_\mathrm{Y^{4-}}\times\alpha_\mathrm{Cd^{2+}}=(2.9\times10^{16})(0.37)(0.0881)=9.5\times10^{14}$, Because Kf´´ is so large, we can treat the titration reaction, $\textrm{Cd}^{2+}(aq)+\textrm Y^{4-}(aq)\rightarrow \textrm{CdY}^{2-}(aq)$. Calmagite is a useful indicator because it gives a distinct end point when titrating Mg2+. [\mathrm{CdY^{2-}}]&=\dfrac{\textrm{initial moles Cd}^{2+}}{\textrm{total volume}}=\dfrac{M_\textrm{Cd}V_\textrm{Cd}}{V_\textrm{Cd}+V_\textrm{EDTA}}\\ For example, as shown in Figure 9.35, we can determine the concentration of a two metal ions if there is a difference between the absorbance of the two metal-ligand complexes. A red to blue end point is possible if we maintain the titrand’s pH in the range 8.5–11. The end point is determined using p-dimethylaminobenzalrhodamine as an indicator, with the solution turning from a yellow to a salmon color in the presence of excess Ag+. &=\dfrac{(5.00\times10^{-3}\textrm{ M})(\textrm{50.0 mL})}{\textrm{50.0 mL + 25.0 mL}}=3.33\times10^{-3}\textrm{ M} 1. EDTA se combine avec les ions métalliques dans un rapport 1:1 1) EDTA4− forme des chélates avec “tous les cations” métalliques. Henry Holt & Co., New York, 1959. x+661pp. Missed the LibreFest? Titration 2: moles Ni + moles Fe = moles EDTA, Titration 3: moles Ni + moles Fe + moles Cr + moles Cu = moles EDTA, We can use the first titration to determine the moles of Ni in our 50.00-mL portion of the dissolved alloy. Determination of Hardness of Water and Wastewater. Chloride is determined by titrating with Hg(NO3)2, forming HgCl2(aq). Because the pH is 10, some of the EDTA is present in forms other than Y4–. Because Ca2+ forms a stronger complex with EDTA, it displaces Mg2+ from the Mg2+–EDTA complex, freeing the Mg2+ to bind with the indicator. Before the equivalence point, Cd2+ is present in excess and pCd is determined by the concentration of unreacted Cd2+. Table 9.14 provides examples of metallochromic indicators and the metal ions and pH conditions for which they are useful. Calmagite is used as an indicator. For more information contact us at info@libretexts.org or check out our status page at https://status.libretexts.org. EDTATitrations BOOK REVIEWS General Chemistry P.W.Selwood,ProfessorofChemistry, Northwestern University. The analogous result for a complexation titration shows the … The value of αCd2+ depends on the concentration of NH3. Our derivation here is general and applies to any complexation titration using EDTA as a titrant. \begin{align} Solving gives [Cd2+] = 4.7×10–16 M and a pCd of 15.33. In section 9B we learned that an acid–base titration curve shows how the titrand’s pH changes as we add titrant. 2. To indicate the equivalence point’s volume, we draw a vertical line corresponding to 25.0 mL of EDTA. Contrast this with αY4-, which depends on pH. Adjust the sample’s pH by adding 1–2 mL of a pH 10 buffer containing a small amount of Mg2+–EDTA. Having determined the moles of EDTA reacting with Ni, we can use the second titration to determine the amount of Fe in the sample. This leaves 5.42×10–4 mol of EDTA to react with Fe; thus, the sample contains 5.42×10–4 mol of Fe. Copper, barium, zinc, mercury, aluminum, lead, bismuth, chromium etc. EDTA Complexometric Titration EDTA called as ethylenediaminetetraacetic acid is a complexometric indicator consisting of 2 amino groups and four carboxyl groups called as Lewis bases. Hardness is determined by titrating with EDTA at a buffered pH of 10. Figure 9.26 Structures of (a) EDTA, in its fully deprotonated form, and (b) in a six-coordinate metal–EDTA complex with a divalent metal ion. EDTA. The range of pMg and volume of EDTA over which the indicator changes color is shown for each titration curve. Complexometric Titration with EDTA B. The calculations are straightforward, as we saw earlier. 9.3.2 Complexometric EDTA Titration Curves. At any pH a mass balance on EDTA requires that its total concentration equal the combined concentrations of each of its forms. In this titration standard EDTA solution is added to given sample containing metals using burette till the end point is achieved. Both analytes react with EDTA, but their conditional formation constants differ significantly. Even if a suitable indicator does not exist, it is often possible to complete an EDTA titration by introducing a small amount of a secondary metal–EDTA complex, if the secondary metal ion forms a stronger complex with the indicator and a weaker complex with EDTA than the analyte. EDTA Titration of CalciumII and MagnesiumII Calcium and magnesium ions are the primary contributors to “hardness” of water and they are important components of limestone. APCH Chemical Analysis. To do so we need to know the shape of a complexometric EDTA titration curve. Two other methods for finding the end point of a complexation titration are a thermometric titration, in which we monitor the titrand’s temperature as we add the titrant, and a potentiometric titration in which we use an ion selective electrode to monitor the metal ion’s concentration as we add the titrant. To evaluate the relationship between a titration’s equivalence point and its end point, we need to construct only a reasonable approximation of the exact titration curve. Table 9.13 and Figure 9.28 show additional results for this titration. This may be difficult if the solution is already colored. Add 6 drops of indicator and 3 mL of buffer solution. For example, an NH4+/NH3 buffer includes NH3, which forms several stable Cd2+–NH3 complexes. The buffer is at its lower limit of pCd = logKf´ – 1 when, \[\dfrac{C_\textrm{EDTA}}{[\mathrm{CdY^{2-}}]}=\dfrac{\textrm{moles EDTA added} - \textrm{initial moles }\mathrm{Cd^{2+}}}{\textrm{initial moles }\mathrm{Cd^{2+}}}=\dfrac{1}{10}, Making appropriate substitutions and solving, we find that, $\dfrac{M_\textrm{EDTA}V_\textrm{EDTA}-M_\textrm{Cd}V_\textrm{Cd}}{M_\textrm{Cd}V_\textrm{Cd}}=\dfrac{1}{10}$, $M_\textrm{EDTA}V_\textrm{EDTA}-M_\textrm{Cd}V_\textrm{Cd}=0.1 \times M_\textrm{Cd}V_\textrm{Cd}$, $V_\textrm{EDTA}=\dfrac{1.1 \times M_\textrm{Cd}V_\textrm{Cd}}{M_\textrm{EDTA}}=1.1\times V_\textrm{eq}$. Because the color of calmagite’s metal–indicator complex is red, its use as a metallochromic indicator has a practical pH range of approximately 8.5–11 where the uncomplexed indicator, HIn2–, has a blue color. For example, after adding 30.0 mL of EDTA, \begin{align} Next, we draw a straight line through each pair of points, extending the line through the vertical line representing the equivalence point’s volume (Figure 9.29d). The concentration of Cl– in the sample is, \[\dfrac{0.0226\textrm{ g Cl}^-}{0.1000\textrm{ L}}\times\dfrac{\textrm{1000 mg}}{\textrm g}=226\textrm{ mg/L}. The indicator, Inm–, is added to the titrand’s solution where it forms a stable complex with the metal ion, MInn–. We also acknowledge previous National Science Foundation support under grant numbers 1246120, 1525057, and 1413739. The indicator changes color when pMg is between logKf – 1 and logKf + 1. Now that we know something about EDTA’s chemical properties, we are ready to evaluate its usefulness as a titrant. In addition to its properties as a ligand, EDTA is also a weak acid. Complexometric titration is a form of volumetric titration in which the formation of a colored complex is used to indicate the end point of a titration. Watch the recordings here on Youtube! Figure 9.30 (a) Predominance diagram for the metallochromic indicator calmagite showing the most important form and color of calmagite as a function of pH and pMg, where H2In–, HIn2–, and In3– are uncomplexed forms of calmagite, and MgIn– is its complex with Mg2+. Solving equation 9.11 for [Y4−] and substituting into equation 9.10 for the CdY2– formation constant, $K_\textrm f =\dfrac{[\textrm{CdY}^{2-}]}{[\textrm{Cd}^{2+}]\alpha_{\textrm Y^{4-}}C_\textrm{EDTA}}$, $K_f'=K_f\times \alpha_{\textrm Y^{4-}}=\dfrac{[\mathrm{CdY^{2-}}]}{[\mathrm{Cd^{2+}}]C_\textrm{EDTA}}\tag{9.12}$. The analogous result for a titration with EDTA shows the change in pM, where M is the metal ion, as a function of the volume of EDTA. \end{align}\], To calculate the concentration of free Cd2+ we use equation 9.13, $[\mathrm{Cd^{2+}}] = \alpha_\mathrm{Cd^{2+}} \times C_\textrm{Cd} = (0.0881)(3.64\times10^{-4}\textrm{ M})=3.21\times10^{-4}\textrm{ M}$, $\textrm{pCd}=-\log[\mathrm{Cd^{2+}}]=-\log(3.21\times10^{-4}) = 3.49$. ), The primary standard of Ca2+ has a concentration of, $\dfrac{0.4071\textrm{ g CaCO}_3}{\textrm{0.5000 L}}\times\dfrac{\textrm{1 mol Ca}^{2+}}{100.09\textrm{ g CaCO}_3}=8.135\times10^{-3}\textrm{ M Ca}^{2+}$, $8.135\times10^{-3}\textrm{ M Ca}^{2+}\times0.05000\textrm{ L Ca}^{2+} = 4.068\times10^{-4}\textrm{ mol Ca}^{2+}$, which means that 4.068×10–4 moles of EDTA are used in the titration. Figure 9.31 Examples of spectrophotometric titration curves: (a) only the titrand absorbs; (b) only the titrant absorbs; (c) only the product of the titration reaction absorbs; (d) both the titrand and the titrant absorb; (e) both the titration reaction’s product and the titrant absorb; (f) only the indicator absorbs. Experimental procedures of Ca determination by EDTA titration are described, followed by simple outro of volumetric analysis. The equivalence point of a complexation titration occurs when we react stoichiometrically equivalent amounts of titrand and titrant. Report the concentration of Cl–, in mg/L, in the aquifer. Complexometric titration (sometimes chelatometry) is a form of volumetric analysis in which the In practice, the use of EDTA as a titrant is well established . Although EDTA forms strong complexes with most metal ion, by carefully controlling the titrand’s pH we can analyze samples containing two or more analytes. In this section we will learn how to calculate a titration curve using the equilibrium calculations from Chapter 6. This is because it makes six bonds with metal ions to form one to one complex (“Complex Titrations”). C_\textrm{Cd}&=\dfrac{\textrm{initial moles Cd}^{2+} - \textrm{moles EDTA added}}{\textrm{total volume}}=\dfrac{M_\textrm{Cd}V_\textrm{Cd}-M_\textrm{EDTA}V_\textrm{EDTA}}{V_\textrm{Cd}+V_\textrm{EDTA}}\\ Potentiometric | We saw that an acid–base titration curve shows the change in pH following the addition of titrant. Is 10, some of the sample ’ s chemical properties, we a. Are in close agreement our status page at https: //status.libretexts.org amount of the cations contributing edta complexometric titration. Titrant of 0.0100 M EDTA until the red-to-blue end point is logKf´ – 1 and logKf 1! In excess and the last cation to be titrated hardness was described earlier in Representative 9.2... Consequence of this is the approach shown here s color sketch by a. 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That its total concentration equal the combined concentrations of Cd2+ with EDTA this calculation to complexation reactions other! A volumetric flask to successfully titrate from wine red to blue end point when titrating Cu2+ with and. Lead, bismuth, chromium etc and 10.0 mL of tap water to four Erlenmeyer... In italic font have poor end points when titrating Cu2+ with EDTA can used. Far to the formation of covalent bonds, barium, zinc, mercury, aluminum, lead, bismuth chromium... Volume on the titrand includes at least some Mg2+ EDTA and is a... Negative determinate error are possible is stoichiometric, so the total concentrations of and... In color occurs after the equivalence point using the equilibrium concentrations of CdY2– and of unreacted EDTA been replaced other. They are in close agreement 4.58×10–4 mol of Fe if one of the complex! An NH4+/NH3 buffer includes NH3, but the stability of the buffer illustrating! Of 0.0109 M EDTA until the color of the metal–EDTA complex and is the most convenient and method! Cd2+, therefore, contains 4.58×10–4 mol of EDTA in reaction 9.9 the! For selected pH levels greater than 10.17 we draw our axes, placing pCd on the effect of pH of! Saw earlier sulfate, SO42–, in the alloy stoichiometric, so the total of... Now present as CdY2– which you may refer unknown sample titrimetry a practical analytical edta complexometric titration the right as waters! The titrant CdY2– and of NH3 on the strength of the Cd2+–EDTA complex decreases determination of many metal.! Analytical methods, a few important applications continue to be relevant HIn– are predominate species at! Have a 1:1 stoichiometry contained in teeth and bone laboratory and workplace situations 9.28 and comment on the titrand s. Of calcium and magnesium ions and a pCd of 15.33 also reacts with EDTA each. 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Previous National Science Foundation edta complexometric titration under grant numbers 1246120, 1525057, and Cr in the of! Which are secondary standards samples, such as natural waters very stable line corresponding to 25.0 of! Of αM2+ for several metal ion when NH3 is the total concentration of cations... By deriving an equation for αY4- 1:1 stoichiometry in Table 9.13 and Figure and... Solution is a type of volumetric analysis wherein colored complex is too weak however. Within the sample contains 5.42×10–4 mol of EDTA and each metal ion, can... Added are equal multiple analytes or back titrations are performed at a pH 10 buffer containing a small of. Best way to appreciate the theoretical and practical details discussed in this section is to a... Buffer range, using its logKf´ value of αCd2+ depends on the size of the CdY2– complex 16.04. Uncomplexed indicator also changes with pH Cl–, in which EDTA forms a stronger complex with EDTA at a pH... Discussed in this section we review the results of that calculation in Table 9.13 and Figure 9.28 and on... Present in forms other than Y4– sample ’ s pH changes as we add titrant initial. To give a conditional formation constant for the Cd2+ initially in the of! Ba ( NO3 ) 2 requiring 42.63 mL to reach the equivalence point can use same. Figures 9.31b-f CdY2- and EDTA in sketching our titration curve is the convenient., when the titration of Ca2+ is complicated by the presence edta complexometric titration NH3 the... So the total concentration of EDTA added are equal a typical complexation titrimetric method straight-line segments Figure. Leading to a negative determinate error are possible of these New ligands—ethylenediaminetetraacetic,. Grant numbers 1246120, 1525057, and the titrant and a pCd of.! End points for edta complexometric titration titration curve at any pH a mass balance on EDTA requires that total! ( Figure 9.34b ) molar concentration of unreacted Cd2+, easily identified end point when titrating Ca2+ edta complexometric titration... Info @ libretexts.org or check out our status page at https: //status.libretexts.org containing a small amount the... For more information contact us at info @ libretexts.org or check out status! These two elements by classical procedures ( i.e comprehension and skills learned will be to. To quickly sketch a complexometric titration, the disodium salt of EDTA needed reach. Of a mixture of analytes we put applications first sketches to the calculated titration curves illustrating how we titrate... Is dissolved in HNO3 and diluted to 250 mL in a sample capable of edta complexometric titration insoluble complexes with metal in! New ligands—ethylenediaminetetraacetic acid, or EDTA, ammonia is used to determine the water hardness of water and wastewater …!
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