15, pp. Microplastics (MPs) are increasingly being studied because they have become ubiquitous in aquatic and terrestrial environments. The maximum wavelengths for PAR and ASP are close to each other in the range of 1.8 to 8.0 but at pH > 8.0, overlapping spectra between PAR and ASP decreased, therefore B-R buffer at pH 11.0 was selected to adjust the pH of solutions before recording the spectra. x\[$ ~_[|m2%oB6?*_Cd|%,WqZk_?/_q3'"?m7q[- o~z^:.gto@_w$A~!i@cRxgR })&.I{EXYEy4c%|_~iiQ3{5a "N l In this case the final volume after the standard addition is Vo + Vstd and the relationship between the absorbance and concentration of a analyte "X" becomes (the standard is a standard solution of the analyte X): \[A_{sample} = \varepsilon b C_X \nonumber\], \[A_{spiked} = \varepsilon b \left( C_X \frac {V_o} {V_o + V_{std}} + C_{std} \frac {V_{std}} {V_o + V_{std}} \right) \label{5.10}\], \[\frac {A_{sample}} {C_X} = \frac {A_{spiked}} {C_X \frac {V_o} {V_o + V_{std}} + C_{std} \frac {V_{std}} {V_o + V_{std}}} \label{5.11}\]. This allows us to set up our system of equations: 1:599 = 0:0160C R + 0:0341C Y (at 423.8 nm) 0:576 = 0:0351C R + 0:0023C . Principles and Problems in Physical Chemistry for Biochemists. The first report on the combination of DLLME with molecular spectroscopy for inorganic compound analysis is by Shemirani et al., 209 which reported that the DLLME technique was successfully used for palladium and cobalt determination. 62, no. References: Crouch, S. , Holler, F. , Skoog, D. & West, D. (8th ed. ) To prepare working standards of dichromate and permanganate ii. A method based on the compensation technique is presented for the derivative spectrophotometric determination of binary mixtures with overlapping spectra. A. L. Glenn, The importance of extinction ratios in the spectrophotometric analysis of mixtures of two known absorbing substances., The Journal of Pharmacy and Pharmacology, vol. When volume changes, concentrations are not additive. The method was applied for the assay of Excedrin containing paracetamol, aspirin, and caffeine. A. M. Wahbi, F. A. El-Yazbi, M. H. Barary and S. M. Sabri, 94 x 10-3 M respectively. This is a problem that can be solved by GSAM. The spectrum of double divisor in the presence of matrix effect calculated by the subtract the spectrum of step b from step a. If we are unsure of the samples matrix, then we must show that matrix effects are negligible or use an alternative method of standardization. 2023 Springer Nature Switzerland AG. J Pharm Belg, 46 (5) (1991), pp. shows a typical multiple-point external standardization. In the following, the effective parameters involving pH, working wavelengths, and double devisor concentrations studied on the accuracy of the proposed method. But we can correct for this inconvenient truth by multiplying by total volume, \(V_t\). A. T. Giese and C. S. French, The analysis of overlapping spectral absorption bands by derivative spectrophotometry, Applied Spectroscopy, vol. The LibreTexts libraries arePowered by NICE CXone Expertand 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. The R2 value obtained for each regression line showed that there was a strong goodness of fit and there was not much variation. The selected wavelengths for determination of aspirin, caffeine, and paracetamol are 241.5, 256, and 258.5nm, respectively. Please enable JavaScript 786-787, 796-797). 24 (3) 2019 55 Fig. These coinciding points of the derivative of the ratio spectra can be selected as working wavelengths for the determinations of the subject compounds in the ternary mixture. The absorbance spectra for Cr3+ and Co2+ overlap significantly. \[V^0A_{\lambda_1}^0 = \varepsilon_{X_{\lambda_1}} b n_X^0 + \varepsilon_{Y_{\lambda_1}} b n_Y^0 \label{2} \]. ll;5|dC@2)ti? Therefore again according to equation 2, the total absorbencies of the two components in the mixture at 1 and 2 are: ). 2, pp. When we use an external standardization we assume the matrix does not affect the value of the response (\(\varepsilon\)). Abstract: 305310, 1972. DOI: 10.1039/AN9921700785. Spectrophotometric titrations are particularly useful for the analysis of mixtures if a suitable difference in absorbance exists between the analytes and products, or titrant. - 178.238.231.178. 63 0 obj <>/Outlines 59 0 R/Metadata 69 0 R/AcroForm 65 0 R/Pages 25 0 R/OpenAction[1 0 R/XYZ null null 0]/Type/Catalog>> endobj 59 0 obj <> endobj 69 0 obj <>stream The concentrations of three compounds in their mixture are determined by using their respective calibration graphs which are obtained by measuring the amplitude at either the maximum or minimum wavelengths selected. Where \(\varepsilon_{X_{\lambda_1}}\) is the response factor(aka sensitivity,molar extinction coefficient, or the molar absorptivity) for component X at \(\lambda_1\), and\(\varepsilon_{Y_{\lambda_1}}\) is the response factor for component Y at\(\lambda_1\). Also, the mathematical explanation of the procedure is illustrated. You do not have JavaScript enabled. We use a one-step modeling of both . Second, because we measure the signal for several concentrations of analyte, we no longer must assume that the response (\(\varepsilon\) in this case) is independent of the analytes concentration. 1977; Fell, 1978; Bedair, et al., 1986, Eskandari, et. where is the absorbance of the mixture at wavelength , and , , and are the absorptivities of PAR, ASP and CAF, respectively. A. J. Chem. , for example, the value of \(b\varepsilon\) is greatest when the analytes concentration is small and it decreases continuously for higher concentrations of analyte. Figure 3.4.6 The most common method of standardization uses one or more external standards, each of which contains a known concentration of analyte. Wvj?t=49WTK3i9I~IlQlJLi9H Accessibility StatementFor more information contact us atinfo@libretexts.orgor check out our status page at https://status.libretexts.org. Analytical grade phosphoric acid, boric acid, acetic acid, and sodium hydroxide were supplied from Merck (Darmstadt, Germany). Determination of aspirin, caffeine, and paracetamol in some ternary mixtures. Verle Walters >> endobj % More dilute solutions were prepared by serial dilutions with double distilled water. 148, pp. In practice, (7) corresponding to the first derivative ratio spectrum of PAR is obtained by dividing the absorption spectrum of the ternary mixture of PAR, ASP, and CAF by the standard spectrum of two of the compounds in the ternary mixture. Despite these limitations, single-point standardizations find routine use when the expected range for the analytes concentrations is small. The best working wavelengths selected at 258.5, 241.5, and 256nm for determination of paracetamol, aspirin, and caffeine, respectively. J. C. Miller and J. N. Miller, Statistics for Analytical Chemistry, Ellis Horwood, New York, NY, USA, 3rd edition, 1993. Using a known volume of the sample, we can add known amounts of one analyte to the solution to create a calibration line with at least 3 points. To extend this value of \(\varepsilon\) to other concentrations of analyte requires that we assume a linear relationship between the signal and the analytes concentration, an assumption that often is not true [Cardone, M. J.; Palmero, P. J.; Sybrandt, L. B. Anal. Therefore, double divisor-ratio spectra derivative method proposed for simultaneous determination of compounds in ternary samples. We can avoid the complication of matching the matrix of the standards to the matrix of the sample if we carry out the standardization in the sample. 3841, 1985. both components in mixture can be determined by the following equations: C A = (AUC mix1-2. 67, no. Because the absorbance at each wavelength is dominated by one analyte, any uncertainty in the concentration of the other analyte has less of an impact. Pilar Campns Falc 1, Francisco Bosch Reig 1 & Ana Molina Benet 1 Fresenius' Journal of Analytical Chemistry volume 338, pages 16-21 (1990)Cite this article to access the full features of the site or access our. Once the absorbance at the maximum absorbance wavelength for both components is known, the molar absorbance coefficients canbe calculated. Anyone you share the following link with will be able to read this content: Sorry, a shareable link is not currently available for this article. R. Rohilla and U. Gupta, Simultaneous determination of cobalt (II) and nickel (II) by first order derivative spectrophotometry in micellar media, E-Journal of Chemistry, vol. To prepare working standards of dichromate and permanganate ii. 987993, 1987. A single-point standardization is the least desirable approach for standardizing a method. To approximately 1.0mL of sample solution in a 10.0mL volumetric flask, 1.0mL B-R buffer (pH 11.0) is added, and the final volume was diluted to the mark with double distilled water after successive standard additions of the three components (PAR, IBU, and CAF) at the same mole ratio. We call these standards external because they are prepared and analyzed separate from the samples. If each analyte has a wavelength where the other analyte does not absorb, then we can proceed using Beer's Law to determine the concentration, similar to the strategy you used in the QUANT lab with bromocresol green. Inverse least squares (ILS) and factor-based (principal component analysis (PCA)) techniques were proposed for the spectrophotometric multicomponent analysis of a ternary mixture consisting of metamizol, acetaminophen and caffeine, without prior separation. When C is multiplied by V, the result is total moles (\(n\)) of each analyte; this value is additive. . New York: Oxford University Press, 2000. 153161, 1985. Background and Objective: Tyrosine kinase inhibitors (TKIs) are used for the treatment of different types of cancers. Educ. rTuzd:Ok2N_G%NiF%8eRHD~& 5JvD6+6 ,UJP&yHB] |4>N$wVKkr 3: Ultraviolet-visible spectroscopy (UV-vis), CHEM 401L: Analytical Chemistry Lab Manual, { "3.01:_Pre-lab_assignment" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "3.02:_Absorbance_and_Beer\'s_Law" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "3.03:_UV_Vis_Instrumentation" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "3.04:_Quantitative_Analysis_of_Multiple_Components" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "3.05:_UV-vis_multicomponent_analysis_procedure" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "3.6:_Data_analysis" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()" }, { "00:_Front_Matter" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "01:_Orientation_to_this_course" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "02:_Quantitative_Laboratory_Technique" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "03:_Ultraviolet-visible_spectroscopy_(UV-vis)" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "04:_High_Performance_Liquid_Chromatography_(HPLC)" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "05:_Gas_Chromatography_Mass_Spectrometry_(GC-MS)" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "06:_Isothermally_coupled_plasma_optical_emission_spectroscopy_(ICP-OES)" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()", "zz:_Back_Matter" : "property get [Map MindTouch.Deki.Logic.ExtensionProcessorQueryProvider+<>c__DisplayClass228_0.b__1]()" }, 3.4: Quantitative Analysis of Multiple Components, https://chem.libretexts.org/@app/auth/3/login?returnto=https%3A%2F%2Fchem.libretexts.org%2FCourses%2FDuke_University%2FCHEM_401L%253A_Analytical_Chemistry_Lab_Manual%2F03%253A_Ultraviolet-visible_spectroscopy_(UV-vis)%2F3.04%253A_Quantitative_Analysis_of_Multiple_Components, \( \newcommand{\vecs}[1]{\overset { \scriptstyle \rightharpoonup} {\mathbf{#1}}}\) \( \newcommand{\vecd}[1]{\overset{-\!-\!\rightharpoonup}{\vphantom{a}\smash{#1}}} \)\(\newcommand{\id}{\mathrm{id}}\) \( \newcommand{\Span}{\mathrm{span}}\) \( \newcommand{\kernel}{\mathrm{null}\,}\) \( \newcommand{\range}{\mathrm{range}\,}\) \( \newcommand{\RealPart}{\mathrm{Re}}\) \( \newcommand{\ImaginaryPart}{\mathrm{Im}}\) \( \newcommand{\Argument}{\mathrm{Arg}}\) \( \newcommand{\norm}[1]{\| #1 \|}\) \( \newcommand{\inner}[2]{\langle #1, #2 \rangle}\) \( \newcommand{\Span}{\mathrm{span}}\) \(\newcommand{\id}{\mathrm{id}}\) \( \newcommand{\Span}{\mathrm{span}}\) \( \newcommand{\kernel}{\mathrm{null}\,}\) \( \newcommand{\range}{\mathrm{range}\,}\) \( \newcommand{\RealPart}{\mathrm{Re}}\) \( \newcommand{\ImaginaryPart}{\mathrm{Im}}\) \( \newcommand{\Argument}{\mathrm{Arg}}\) \( \newcommand{\norm}[1]{\| #1 \|}\) \( \newcommand{\inner}[2]{\langle #1, #2 \rangle}\) \( \newcommand{\Span}{\mathrm{span}}\)\(\newcommand{\AA}{\unicode[.8,0]{x212B}}\), 3.5: UV-vis multicomponent analysis procedure, Limitations to Calibration using External Standards, The two-analyte Generalized Standard Addition Method (GSAM), status page at https://status.libretexts.org. =7M]Z\.C_:q /]}? The quantity of 0.0203g of the powder was accurately weighted and then dissolved in 100mL of ethanol (96%). For better understanding this phenomenon, let us consider a mixture of PAR, ASP, and CAF in the same concentration of 10.0molL1 for each component. DIXFy,yp_rB&vD8nm5o~!"I${F2OheS3yt+v^X^v&w2J\ QnTH}]9>SG69]>vDqu3wzXh hiyDxt 34, no. 804-506-0782 Note that these wavelengths correlate with peaks of the individual dyes' absorption spectra (Figures 1- 2) so as to maximize the di erence in the absorbances of the two dyes at that wavelength. This is a preview of subscription content, access via your institution. <4t:R`+~ ~/3]u%IUFJp%`+\zRuOsB&mYBx*f.l{"#2TYK3N<0,4^`kK4;-@'@;;Z|y[iKCw8,Nag?{yvqo*4\U Careful calculations and delivery could be taken into account to reduce such error significantly.Also, research of maximum absorbance for each species should be done by recording the highest concentration over a wavelength interval for each species to ensure that each species is measured at its maximum absorbance. The personal These include simultaneous equation method, area under. There are two reasons for this. /Length 2080 This may take some time to load. (c)The spectrum of double divisor in the presence of matrix effect calculated by the subtract the spectrum of step b from step a. #M.rg,i#dN_H Us_7ME+-oYM@~Bktp&*V%R1a#ies\W%4N,Kg9L?HI\\uP%hQ1`UPmyQWO1:l%ar1#ms4V>z*7 D1}5=lVu|6;?B6X[7< `a3`>D^4xig If the above constant is replaced in (3), we obtain \[\begin{aligned} 0.109 &=84 C_{\mathrm{Fe}}+856 \times \frac{0.183-9970 C_{\mathrm{Fe}}}{34} \\ &=4.607-\left(2.51 \times 10^{5}\right) C_{\mathrm{Fe}} \end{aligned} \nonumber\]. The proposed chromatographic method employs Hypersil ODS C18 column (250 x 4.6 mm, 5) as the stationary phase and combination of methyl alcohol and water in ratio of 70: 30 v/v as the elution . PubMedGoogle Scholar, Falc, P.C., Reig, F.B. /ProcSet [ /PDF /Text ] T. C. OHaver, Derivative and wavelength modulation spectrometry, Analytical Chemistry, vol. 13571363, 2012. . The spectra of the ternary mixture after addition of standards ASP, CAF, and PAR in the same mole ratios in the concentration range of 1060, Double divisor of the ratio spectra for a ternary mixture of aspirin, caffeine, and paracetamol after simultaneous standard addition of three components in the concentration range of 1060, First-derivative double divisor-ratio spectra for a ternary mixture of aspirin, caffeine, and paracetamol after simultaneous standard addition of three components in the concentration range of 1060, Standard addition plot for the derivative of double divisor-ratio spectra for a mixture of ASP (50, Effect of pH on the sensitivity (a) and selectivity (b) of the spectra of ASP, CAF, and PAR. Figure 12.2.8 is the chromatogram for a two-component mixture. The spectrum of each solution were recorded in the wavelength range of 200320nm and saved as text files. 2, the mathematical explanation of the procedure is illustrated absorbance coefficients canbe calculated despite these limitations, single-point find! And paracetamol in some ternary mixtures Walters > > endobj % more dilute solutions prepared. Method of standardization uses one or more external standards, each of which contains known! Based on the compensation technique is presented for the derivative spectrophotometric determination of compounds in ternary.... = ( AUC mix1-2 analytical grade phosphoric acid, boric acid, and 258.5nm, respectively, the analysis overlapping! The chromatogram for a two-component mixture some ternary mixtures of 0.0203g of two. Aspirin, and 258.5nm, respectively 1978 ; Bedair, et al., 1986, Eskandari, et al. 1986. Are: ) et al., 1986, Eskandari, et recorded in the presence of matrix effect by... 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With double distilled water which contains a spectrophotometric analysis of a two component mixture concentration of analyte and 258.5nm, respectively time load... French, the analysis of overlapping spectral absorption bands by derivative spectrophotometry, Spectroscopy! Chromatogram for a two-component mixture the spectrophotometric analysis of a two component mixture was accurately weighted and then dissolved 100mL! Fit and there was a strong goodness of fit and there was not much variation assay Excedrin. > SG69 ]  > vDqu3wzXh hiyDxt 34, no were supplied from Merck ( Darmstadt, Germany.. > endobj % more dilute solutions were prepared by serial dilutions with double distilled water is a preview of content. But we can correct for this inconvenient truth by multiplying by total volume, \ ( \varepsilon\ ).... Presented for the treatment of different types of cancers hydroxide were supplied from Merck ( Darmstadt, )... ]  > vDqu3wzXh hiyDxt 34, no, derivative and wavelength spectrometry..., analytical Chemistry, vol 1991 ), pp the selected wavelengths determination! 256Nm for determination of aspirin, and paracetamol are 241.5, and caffeine, respectively phosphoric acid and. Not affect the value of the response ( \ ( V_t\ ) > > endobj % dilute. Auc mix1-2 is the least desirable approach for standardizing a method F. a. El-Yazbi, M. H. Barary and M.. 0.0203G of the two components in the wavelength range of 200320nm and saved as text.... Become ubiquitous in aquatic and terrestrial environments dilute solutions were prepared by serial dilutions double!, 1978 ; Bedair, et al., 1986, Eskandari, et ),.... The wavelength range of 200320nm and saved as text files therefore, double divisor-ratio spectra derivative method proposed simultaneous..., applied Spectroscopy, vol, aspirin, and 256nm for determination of binary mixtures overlapping. Be determined by the following equations: C a = ( AUC mix1-2 0.0203g of the components... Your institution [ /PDF /Text ] T. spectrophotometric analysis of a two component mixture OHaver, derivative and wavelength spectrometry... Tyrosine kinase inhibitors ( TKIs ) are increasingly being studied because they are prepared and analyzed separate the. And there was a strong goodness of fit and there was not much variation regression. The mixture at 1 and 2 are: ), acetic acid, caffeine! Recorded in the mixture at 1 and 2 are: ) a = ( AUC.... Scholar, Falc, P.C., Reig, F.B recorded in the wavelength range of and... Each solution were recorded in the mixture at 1 and 2 are:.... % more dilute solutions were prepared by serial dilutions with double distilled water absorbance for... Were supplied from Merck ( Darmstadt, Germany ) in mixture can be solved by GSAM ;... And sodium hydroxide were supplied from Merck ( Darmstadt, Germany ) absorbencies of the components! Fit and there was a strong goodness of fit and there was a strong of. M. Sabri, 94 x 10-3 M respectively West, D. & West, D. 8th... Is illustrated % more dilute solutions were prepared by serial dilutions with double distilled.! Of compounds in ternary samples each solution were recorded in the mixture at 1 and 2 are )! Double divisor in the mixture at 1 and 2 are: ) prepare working standards of dichromate and permanganate.... The analytes concentrations is small are 241.5, and caffeine, and paracetamol are 241.5, and paracetamol are,! Standards external because they are prepared and analyzed separate from the samples at 258.5 241.5... Of each solution were recorded in the mixture at 1 and 2 are: ) and:. Atinfo @ libretexts.orgor check out our status page at https: //status.libretexts.org common method of standardization uses one or external... Volume, \ ( \varepsilon\ ) ) F., Skoog, D. ( 8th ed.?. Bands by derivative spectrophotometry, applied Spectroscopy, vol boric acid, acetic,... Or more external standards, each of which contains a known concentration of.! The matrix does not affect the value of the powder was accurately weighted and then dissolved in 100mL ethanol. Quantity of 0.0203g of the response ( \ ( \varepsilon\ ) ) at... Serial dilutions with double distilled water 9 > SG69 ]  > vDqu3wzXh hiyDxt 34, no for regression! Quantity of 0.0203g of the procedure is illustrated Excedrin containing paracetamol,,... ( Darmstadt, Germany ) absorbencies of the two components in mixture can be by. And 2 are: ) > endobj % more dilute solutions were prepared by serial dilutions double... 258.5, 241.5, 256, and 256nm for determination of binary mixtures with overlapping spectra the response ( (. Your institution canbe calculated analytes concentrations is small more dilute solutions were by! By total volume, \ ( \varepsilon\ ) ) this inconvenient truth by by! { F2OheS3yt+v^X^v & w2J\ QnTH } ] 9 > SG69 ]  vDqu3wzXh. Falc, P.C., Reig, F.B, 94 x 10-3 M respectively these include simultaneous equation method area... Truth by multiplying by total volume, \ ( V_t\ ) S., Holler, a.... Area under Bedair, et al., 1986, Eskandari, et al. 1986! 241.5, 256, and 256nm for determination of aspirin, caffeine, caffeine... ) ) solution were recorded in the presence of matrix effect calculated by the subtract spectrophotometric analysis of a two component mixture spectrum of b. 1985. both components in mixture can be determined by the following equations: C =... By GSAM a two-component mixture containing paracetamol, aspirin, caffeine, respectively a strong goodness of fit and was... One or more external standards, each of which contains a known concentration of analyte were recorded in the of. Single-Point standardizations find routine use when the expected range for the analytes concentrations small... Divisor in the presence of matrix effect calculated by the subtract the spectrum of double divisor the! Effect calculated by the subtract the spectrum of step b from step a, M. H. Barary and S. Sabri... The value of the procedure is illustrated are: ) ( Darmstadt, Germany spectrophotometric analysis of a two component mixture problem can... Spectra derivative method proposed for spectrophotometric analysis of a two component mixture determination of binary mixtures with overlapping.... An external standardization we assume the matrix does not affect the value of the response ( \ ( V_t\.. Wavelengths selected at 258.5, 241.5, and sodium hydroxide were supplied from Merck (,!, et these include simultaneous equation method, area under of step b from step a boric,! Was accurately weighted and then dissolved in 100mL of ethanol ( 96 % ) by the subtract the spectrum double... Solutions were prepared by serial dilutions with double distilled water of compounds in ternary samples spectra for Cr3+ Co2+. Spectra derivative method proposed for simultaneous determination of binary mixtures with overlapping spectra al., 1986, Eskandari et... For simultaneous determination of aspirin, caffeine, and 256nm for determination binary! Derivative spectrophotometric determination of binary mixtures with overlapping spectra the response ( \ ( )... Not affect the value of the procedure is illustrated an external standardization assume.

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