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US4734376A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the spectrophotometric measurement of lithium ion employing a chromogenic aza-12-crown-4- ether

Assignee: University of Miami
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Filing: 1986-10-22
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Granted: 1988-03-29
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Expires: 2006-10-22
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Abstract

Abstract Chromogenic aza-12-crown-4 ethers which can be used for the spectrophotometric determination of lithium ion in aqueous solutions are disclosed. The compounds of the invention are particularly useful for the analysis of Li + in the presence of Na + , a situation common in biological and geological systems. The compounds [e.g., 1-(2-oxy-5-nitrobenzyl)-1-hydro-1-aza-4,7,10-trioxacyclododecane], their methods of manufacture, and methods of utilizing the compounds for the analysis of lithium are disclosed.

Inventors

  • 👤 Gilbert E. Pacey
  • 👤 Ken-ichi Sasaki

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 23:39
CPC Classifications
C; C07; C07D; C07D273/00; Y; Y10; Y10T; Y10T436/00; Y10T436/25; Y10T436/25375; Y10T436/255

Claims Analysis

Total Claims: 13
Claim 1
Independent Claim 204 words
A process for the spectrophotometric determination of the concentration of lithium ions in an aqueous solution, said process comprising the following steps: (a) mixing in a common vessel: (i) a measured quantity of a lithium-ion-containing aqueous solution; and (ii) a measured quantity of the crown ether compound ##STR5## (b) combining said aqueous solution with a measured quantity of a hydroxide containing base; (c) adding a measured amount of a water-immiscible organic solvent to said vessel whereby an aqueous phase and an organic phase are formed; (d) agitating said vessel to extract any material soluble in said organic solvent into said organic phase; (e) transferring a measured quantity of said organic phase into a first spectrophotometric cell and a quantity of a reagent blank into a second spectrophotometric cell; (f) scanning said cells with ultraviolet-visible light and recording the relative light absorbance of said organic phase with respect to said reagent blank at a wavelength of approximately 400 nm; and (g) determining the concentration of lithium ions in said aqueous solution by comparing said relative absorbance with the relative absorbance at the same wavelength or organic phases obtained by treating aqueous solutions containing known concentrations of lithium ions in accordance with steps a through f.
Claim 2
Dependent Claim 204 words
A process for the spectrophotometric determination of the concentration of lithium ions in an aqueous solution, said process comprising the following steps: (a) mixing in a common vessel: (i) a measured quantity of a lithium-ion-containing aqueous solution; and (ii) a measured quantity of the crown ether compound ##STR5## (b) combining said aqueous solution with a measured quantity of a hydroxide containing base; (c) adding a measured amount of a water-immiscible organic solvent to said vessel whereby an aqueous phase and an organic phase are formed; (d) agitating said vessel to extract any material soluble in said organic solvent into said organic phase; (e) transferring a measured quantity of said organic phase into a first spectrophotometric cell and a quantity of a reagent blank into a second spectrophotometric cell; (f) scanning said cells with ultraviolet-visible light and recording the relative light absorbance of said organic phase with respect to said reagent blank at a wavelength of approximately 400 nm; and (g) determining the concentration of lithium ions in said aqueous solution by comparing said relative absorbance with the relative absorbance at the same wavelength or organic phases obtained by treating aqueous solutions containing known concentrations of lithium ions in accordance with steps a through f.
Claim 3
Dependent Claim 22 words
The process of claim 1 wherein said organic solvent is selected from the group consisting of methylene chloride, chloroform and 1, 2-dichloroethane.
Claim 4
Dependent Claim 28 words
The process of claim 1 wherein the amount of said organic solvent added to said vessel is substantially equal in volume to the aqueous solution in said vessel.
Claim 5
Dependent Claim 20 words
The process of claim 1 wherein said base is selected from the group consisting of potassium hydroxide and sodium hydroxide.
Claim 6
Dependent Claim 77 words
The process of claim 1 wherein said scanning step comprises: (i) providing a light source which is capable of emitting radiation covering the wavelength range of 250 nm through approximately 500 nm; (ii) beaming radiation from said light source through said spectrophotometric cells while varying the wavelength thereof throughout the range 250 nm to approximately 500 nm; and (iii) recording the absorbance of said radiation of said organic phase and said reagent blank throughout said wavelength range.
Claim 7
Dependent Claim 11 words
The process of claim 1 wherein said organic solvent is chloroform.
Claim 8
Dependent Claim 24 words
The process of claim 6 wherein the chloroform includes an amount of t-butyl alcohol improve the stability of the absorbance of the organic phase.
Claim 9
Dependent Claim 206 words
A process for the spectrophotometric determination of the concentration of lithium ions in an aqueous solution, said process comprising the following steps: (a) mixing in a common vessel: (i) a measured quantity of a lithium-ion-containing aqueous soltuion; and (ii) a measured quantity of the crown ether compound ##STR6## (b) combining said aqueous soltuion with a measured quantity of a base selected from the group consisting of sodium hydroxide and potassium hydroxide; (c) adding a measured amount of chloroform to said vessel whereby an aqueous phase and an organic phase are formed; (d) agitating said vessel to extract any material soluble in chloroform into said organic phase; (e) transferring a measured quantity of said organic phase into a first spectrophotometric cell and a quantity of a reagent blank into a second spectrophotometric cell; (f) scanning said cells with ultraviolet-visible light and recording the relative light absorbance of said organic phase with respect to said reagent blank at a wavelength of approximately 400 nm; and (g) determining the concentration of lithium ions in said aqueous solution by comparing said relative absorbance with the relative absorbance at the same wavelength of solutions containing known concentrations of lithium ions which have been treated in accordance with steps a through f.
Claim 10
Dependent Claim 206 words
A process for the spectrophotometric determination of the concentration of lithium ions in an aqueous solution, said process comprising the following steps: (a) mixing in a common vessel: (i) a measured quantity of a lithium-ion-containing aqueous soltuion; and (ii) a measured quantity of the crown ether compound ##STR6## (b) combining said aqueous soltuion with a measured quantity of a base selected from the group consisting of sodium hydroxide and potassium hydroxide; (c) adding a measured amount of chloroform to said vessel whereby an aqueous phase and an organic phase are formed; (d) agitating said vessel to extract any material soluble in chloroform into said organic phase; (e) transferring a measured quantity of said organic phase into a first spectrophotometric cell and a quantity of a reagent blank into a second spectrophotometric cell; (f) scanning said cells with ultraviolet-visible light and recording the relative light absorbance of said organic phase with respect to said reagent blank at a wavelength of approximately 400 nm; and (g) determining the concentration of lithium ions in said aqueous solution by comparing said relative absorbance with the relative absorbance at the same wavelength of solutions containing known concentrations of lithium ions which have been treated in accordance with steps a through f.
Claim 11
Dependent Claim 26 words
The process of claim 8 wherein said chloroform includes an amount of t-butyl alcohol sufficient to improve the stability of the absorbance of the organic phase.
Claim 12
Dependent Claim 26 words
The process of claim 8 wherein the amount of chloroform added to said vessel is substantially equal in volume to the aqueous solution in said vessel.
Claim 13
Dependent Claim 78 words
The process of claim 8 wherein said scanning step comprises: (i) providing a light source which is capable of emitting radiation covering the wavelength range of 250 nm through approximately 500 nm; (ii) beaming radiation from said light source through said spectrophotometric cells while varying the wavelength thereof throughout the range of 250 nm to approximately 500 nm; and (iii) recording the absorbance of said radiation by said organic phase and said reagent blank through said wavelength range.

References Cited (Backward Citations)

US4367072A Cited
US4436923A Cited
EP0125555A2 Cited
US4645744A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1991-03-29 1991-09-28 1992-03-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1995-03-29 1995-09-28 1996-03-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1999-03-29 1999-09-28 2000-03-29 $7700.00 Window Closed / Lapsed

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