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Nitrilotris(methylenephosphonates) in aqueous solution and solid state – dilatometric, potentiometric and NMR investigations.

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Title: Nitrilotris(methylenephosphonates) in aqueous solution and solid state – dilatometric, potentiometric and NMR investigations.
Authors: Grossmann, Gisbert1 Gisbert.Grossmann@t-online.de, Burkov, Kim A.2, Hägele, Gerhard3, Myund, Lubov A.2, Hermens, Stephan3, Verwey, Claudia3, Arat-ool, Sholban M.2
Source: Inorganica Chimica Acta. Feb2004, Vol. 357 Issue 3, p797-808. 12p.
Subjects: Phosphonates, Nuclear magnetic resonance, Volumetric analysis, Dilatometers
Abstract: Dissociation and alkali complex formation equilibria of nitrilotris(methylenephosphonic acid) (NTMP, H6L) have been studied by dilatometric, potentiometric and 31P NMR-controlled titrations. Dilatometry indicated the formation of alkali complexes ML (M=Li, Na, K, Rb, Cs) at high pH with a stability decreasing from Li to Cs. An efficient combination of potentiometric and NMR methods confirmed two types of alkali metal complexes MHL and ML. Stability constants for the equilibria following M+ + HL5− ⇌ MHL4− and M+ + L6− ⇌ ML5−, respectively, were determined: logKNaHL=1.08(0.07), logKKHL=0.86(0.08), logKNaL=2.24(0.03). Systematic errors are introduced by using alkali metal hydroxides as titrants for routine potentiometric determinations of dissociation constants pKa5app and pKa6app. Correction formulae were derived to convert actual dissociation constants pKa into apparent dissociation constants pKaapp (or vice versa). The actual dissociation constants were found: pKa5(H2L4− ⇌ H+ + HL5−)=7.47(0.03) and pKa6(HL5− ⇌ H+ + L6−)=14.1(0.1). The anisotropy of 31P chemical shifts of salts MnH6 − nL (M=Li, Na, n=0–5) is more sensitive towards titration (n) than isotropic solution state chemical shifts.Results obtained by potentiometric and NMR-controlled titrations of nitrilotris(methylenephosphonic acid) (NTMP, H6L) with tetramethylammonium hydroxide (TMAOH) in the presence of NaCl clearly indicate the formation of complexes NaL5− and NaHL4−. Dilatometric titrations of NTMP using the hydroxides of Li, Na, K, Rb, and Cs indicate that the tendency to form complexes between alkali cations and L6− decreases from Li to Cs. [Copyright &y& Elsevier]
Copyright of Inorganica Chimica Acta is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: Nitrilotris(methylenephosphonates) in aqueous solution and solid state – dilatometric, potentiometric and NMR investigations.
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  Data: <searchLink fieldCode="AR" term="%22Grossmann%2C+Gisbert%22">Grossmann, Gisbert</searchLink><relatesTo>1</relatesTo><i> Gisbert.Grossmann@t-online.de</i><br /><searchLink fieldCode="AR" term="%22Burkov%2C+Kim+A%2E%22">Burkov, Kim A.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Hägele%2C+Gerhard%22">Hägele, Gerhard</searchLink><relatesTo>3</relatesTo><br /><searchLink fieldCode="AR" term="%22Myund%2C+Lubov+A%2E%22">Myund, Lubov A.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Hermens%2C+Stephan%22">Hermens, Stephan</searchLink><relatesTo>3</relatesTo><br /><searchLink fieldCode="AR" term="%22Verwey%2C+Claudia%22">Verwey, Claudia</searchLink><relatesTo>3</relatesTo><br /><searchLink fieldCode="AR" term="%22Arat-ool%2C+Sholban+M%2E%22">Arat-ool, Sholban M.</searchLink><relatesTo>2</relatesTo>
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  Data: <searchLink fieldCode="JN" term="%22Inorganica+Chimica+Acta%22">Inorganica Chimica Acta</searchLink>. Feb2004, Vol. 357 Issue 3, p797-808. 12p.
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  Data: <searchLink fieldCode="DE" term="%22Phosphonates%22">Phosphonates</searchLink><br /><searchLink fieldCode="DE" term="%22Nuclear+magnetic+resonance%22">Nuclear magnetic resonance</searchLink><br /><searchLink fieldCode="DE" term="%22Volumetric+analysis%22">Volumetric analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Dilatometers%22">Dilatometers</searchLink>
– Name: Abstract
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  Data: Dissociation and alkali complex formation equilibria of nitrilotris(methylenephosphonic acid) (NTMP, H6L) have been studied by dilatometric, potentiometric and 31P NMR-controlled titrations. Dilatometry indicated the formation of alkali complexes ML (M=Li, Na, K, Rb, Cs) at high pH with a stability decreasing from Li to Cs. An efficient combination of potentiometric and NMR methods confirmed two types of alkali metal complexes MHL and ML. Stability constants for the equilibria following M+ + HL5− ⇌ MHL4− and M+ + L6− ⇌ ML5−, respectively, were determined: logKNaHL=1.08(0.07), logKKHL=0.86(0.08), logKNaL=2.24(0.03). Systematic errors are introduced by using alkali metal hydroxides as titrants for routine potentiometric determinations of dissociation constants pKa5app and pKa6app. Correction formulae were derived to convert actual dissociation constants pKa into apparent dissociation constants pKaapp (or vice versa). The actual dissociation constants were found: pKa5(H2L4− ⇌ H+ + HL5−)=7.47(0.03) and pKa6(HL5− ⇌ H+ + L6−)=14.1(0.1). The anisotropy of 31P chemical shifts of salts MnH6 − nL (M=Li, Na, n=0–5) is more sensitive towards titration (n) than isotropic solution state chemical shifts.Results obtained by potentiometric and NMR-controlled titrations of nitrilotris(methylenephosphonic acid) (NTMP, H6L) with tetramethylammonium hydroxide (TMAOH) in the presence of NaCl clearly indicate the formation of complexes NaL5− and NaHL4−. Dilatometric titrations of NTMP using the hydroxides of Li, Na, K, Rb, and Cs indicate that the tendency to form complexes between alkali cations and L6− decreases from Li to Cs. [Copyright &y& Elsevier]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Inorganica Chimica Acta is the property of Elsevier B.V. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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        Value: 10.1016/j.ica.2003.09.011
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      – Code: eng
        Text: English
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        PageCount: 12
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      – SubjectFull: Phosphonates
        Type: general
      – SubjectFull: Nuclear magnetic resonance
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      – SubjectFull: Volumetric analysis
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      – SubjectFull: Dilatometers
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      – TitleFull: Nitrilotris(methylenephosphonates) in aqueous solution and solid state – dilatometric, potentiometric and NMR investigations.
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              Text: Feb2004
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              Y: 2004
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