US4699718A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Ion chromatography method and apparatus
Assignee: Waters Technologies Corp
•
Filing: 1986-01-21
•
Granted: 1987-10-13
•
Expires: 2006-01-21
Abstract
Abstract A method and apparatus for the simultaneous analysis of borate and chloride ions in a liquid sample, such as a sample of nuclear reactor water, by ion chromatographic techniques are disclosed. The ion chromatographic system employed includes an exclusion column, an anion exchange column, and means for alternately directing effluent from said exclusion column to refractive index detecting means or void volume from the exclusion column and second eluent through the anion exchange column to conductivity detecting means.
Inventors
- 👤 William R. Jones
- 👤 Allan L. Heckenberg
- 👤 Petr Jandik
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 02:17
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/96
Claims Analysis
Total Claims: 25
Claim 1
Independent Claim
162 words
A method for the simultaneous chromatographic separation and quantitative analysis of weakly ionized anions and strongly ionized anions in a liquid sample, comprising: (a) eluting the liquid sample and a first eluent through a liquid chromatographic exclusion column packed with exclusion resin capable of resolving weakly ionized anions in effluent from the exclusion column and passing strongly ionized anions in void volume from the exclusion column; (b) simultaneously eluting void volume containing the strongly ionized anions from said chromatographic exclusion column and a second eluent through a liquid chromatographic anion column packed with an anion resin capable of resolving said strongly ionized anions in effluent from said anion column; (c) detecting and monitoring the refractive index of effluent from said exclusion column as an indication of the quantity of weakly ionized anions in the sample; and (d) detecting and monitoring the electrical conductivity of effluent from said anion column as an indication of the quantity of strongly ionized anions in the sample.
Claim 2
Independent Claim
162 words
A method for the simultaneous chromatographic separation and quantitative analysis of weakly ionized anions and strongly ionized anions in a liquid sample, comprising: (a) eluting the liquid sample and a first eluent through a liquid chromatographic exclusion column packed with exclusion resin capable of resolving weakly ionized anions in effluent from the exclusion column and passing strongly ionized anions in void volume from the exclusion column; (b) simultaneously eluting void volume containing the strongly ionized anions from said chromatographic exclusion column and a second eluent through a liquid chromatographic anion column packed with an anion resin capable of resolving said strongly ionized anions in effluent from said anion column; (c) detecting and monitoring the refractive index of effluent from said exclusion column as an indication of the quantity of weakly ionized anions in the sample; and (d) detecting and monitoring the electrical conductivity of effluent from said anion column as an indication of the quantity of strongly ionized anions in the sample.
Claim 3
Dependent Claim
12 words
A method of claim 1 wherein said weakly ionized anions include borate.
Claim 4
Dependent Claim
12 words
A method of claim 2 wherein said strongly ionized anions include chloride.
Claim 5
Dependent Claim
13 words
A method of claim 3 wherein said first eluent comprises an inorganic acid.
Claim 6
Dependent Claim
19 words
A method of claim 3 wherein said first eluent comprises an aqueous solution of alkyl or aryl sulfonic acid.
Claim 7
Dependent Claim
20 words
A method of claim 5 wherein said second eluent comprises an aqueous solution of a carborylic acid or salt thereof.
Claim 8
Dependent Claim
21 words
A method of claim 6 wherein said second eluent comprises an aqueous solution of sodium or potassium alkyl or aryl sulfonate.
Claim 9
Dependent Claim
20 words
A method of claim 3 wherein said second eluent comprises an aqueous solution of a carborylic acid or salt thereof.
Claim 10
Dependent Claim
183 words
In the quantitative analysis of borate ions and chloride ions in a sample of nuclear reactor water including the steps of resolving the borate ions present in said sample in a first chromatographic separation and resolving chloride ions in a second chromatographic separation: the improvement comprising performing both chromatographic separations on-line and simultaneously by: (a) eluting a sample of the nuclear reactor water with a first eluent through a chromatgraphic exclusion column under conditions whereby chloride ions in the sample exit the column in its void volume and boric acid present in the sample are resolved in effluent from the exclusion column; (b) eluting void volume from said chromatographic exclusion column with a second eluent through a chromatographic anion column under conditions whereby chloride ions in said sample are resolved in effluent from the anion column; and (c) simultaneously monitoring the refractive index of effluent from the exclusion column as an indication of the amount of borate ions in the sample and the electrical conductivity of effluent from the anion column as an indication of the quantity of chloride ions in the sample.
Claim 11
Dependent Claim
183 words
In the quantitative analysis of borate ions and chloride ions in a sample of nuclear reactor water including the steps of resolving the borate ions present in said sample in a first chromatographic separation and resolving chloride ions in a second chromatographic separation: the improvement comprising performing both chromatographic separations on-line and simultaneously by: (a) eluting a sample of the nuclear reactor water with a first eluent through a chromatgraphic exclusion column under conditions whereby chloride ions in the sample exit the column in its void volume and boric acid present in the sample are resolved in effluent from the exclusion column; (b) eluting void volume from said chromatographic exclusion column with a second eluent through a chromatographic anion column under conditions whereby chloride ions in said sample are resolved in effluent from the anion column; and (c) simultaneously monitoring the refractive index of effluent from the exclusion column as an indication of the amount of borate ions in the sample and the electrical conductivity of effluent from the anion column as an indication of the quantity of chloride ions in the sample.
Claim 12
Dependent Claim
16 words
The improvement of claim 9 wherein said first eluent comprises an alkyl or aryl sulfonic acid.
Claim 13
Dependent Claim
17 words
The improvement of claim 10 wherein said second eluent comprises sodium or potassium alkyl or aryl sulfonate.
Claim 14
Independent Claim
181 words
An apparatus for the chromatographic separation and quantitative analysis of weakly ionized anions and strongly ionized anions in a liquid sample, comprising: (a) a chromatographic exclusion column packed with an exclusion resing capable of resolving weakly ionized anions in effluent from said exclusion column and passing strongly ionized anions in void volume from said exclusion column; (b) a reservoir of first eluent; (c) a means for pumping first eluent through said chromatographic exclusion column; (d) sample injection means for injection a liquid sample containing weakly ionized anions and strongly ionized anions into first eluent prior to said chromatographic exclusion column; (e) refractive index monitoring means for monitoring the refractive index of effluent containing weakly ionized anions from said chromatographic exclusion column; (f) a chromatographic anion column packed with an anion exchange resin capable of resolving strongly ionized anions in effluent from said anion column; (g) a reservoir of second eluent; (h) means for pumping second eluent through said chromatographic anion column; (i) conductivity monitoring means for monitoring the electrical conductivity of effluent containing strongly ionized anions from said chromatographic anion column;
Claim 15
Independent Claim
181 words
An apparatus for the chromatographic separation and quantitative analysis of weakly ionized anions and strongly ionized anions in a liquid sample, comprising: (a) a chromatographic exclusion column packed with an exclusion resing capable of resolving weakly ionized anions in effluent from said exclusion column and passing strongly ionized anions in void volume from said exclusion column; (b) a reservoir of first eluent; (c) a means for pumping first eluent through said chromatographic exclusion column; (d) sample injection means for injection a liquid sample containing weakly ionized anions and strongly ionized anions into first eluent prior to said chromatographic exclusion column; (e) refractive index monitoring means for monitoring the refractive index of effluent containing weakly ionized anions from said chromatographic exclusion column; (f) a chromatographic anion column packed with an anion exchange resin capable of resolving strongly ionized anions in effluent from said anion column; (g) a reservoir of second eluent; (h) means for pumping second eluent through said chromatographic anion column; (i) conductivity monitoring means for monitoring the electrical conductivity of effluent containing strongly ionized anions from said chromatographic anion column;
Claim 16
Dependent Claim
34 words
(j) means for alternately directing void volume from the chromatographic exclusion column and second effluent to said chromatographic anion column or directing effluent from said chromatographic exclusion column to said refractive index monitoring means;
Claim 17
Dependent Claim
34 words
(j) means for alternately directing void volume from the chromatographic exclusion column and second effluent to said chromatographic anion column or directing effluent from said chromatographic exclusion column to said refractive index monitoring means;
Claim 18
Dependent Claim
37 words
(k) control means for operating said valve alternately to direct void volume from said exclusion column and second effluent to said chromatograhic anion column and effluent from said chromatographic exclusion column to said refractive index monitoring means.
Claim 19
Dependent Claim
37 words
(k) control means for operating said valve alternately to direct void volume from said exclusion column and second effluent to said chromatograhic anion column and effluent from said chromatographic exclusion column to said refractive index monitoring means.
Claim 20
Dependent Claim
19 words
An apparatus of claim 12 wherein said exclusion resin is capable of resolving boric acid present in said sample.
Claim 21
Dependent Claim
20 words
An apparatus of claim 13 wherein said anion exchange resin is capable of resolving chloride ions present in said sample.
Claim 22
Dependent Claim
13 words
An apparatus of claim 14 wherein said exclusion resin comprises a sulfonated polymer.
Claim 23
Dependent Claim
18 words
An apparatus of claim 15 wherein said sulfonated polymer comprises a sulfonated copolymer of styrene and divinyl benzene.
Claim 24
Dependent Claim
21 words
An apparatus of claim 12 wherein said sample injection means comprises means for injecting a sample of predetermined or variable volume.
Claim 25
Dependent Claim
19 words
An apparatus of claim 17 wherein said means for alternately directing comprises a valve having at least six ports.
References Cited (Backward Citations)
US3920397A
Cited
US3926559A
Cited
US3966596A
Cited
US4073725A
Cited
US4314823A
Cited
US4507390A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-10-12 | 1991-04-13 | 1991-10-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-10-12 | 1995-04-13 | 1995-10-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-10-12 | 1999-04-13 | 1999-10-13 | $7700.00 | Window Closed / Lapsed |