US4629566A
Expired / Lapsed
US
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Method for characterizing the molecular weight and molecular weight distribution of ultra-high molecular weight water soluble polymers
Assignee: Dow Chemical Co
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Filing: 1985-05-24
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Granted: 1986-12-16
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Expires: 2005-05-24
Abstract
Abstract The molecular weight and molecular weight distribution of diverse ultra-high molecular weight water soluble polymers is rapidly determined based on apparent size by passage of extremely dilute samples of the polymer (1-250 ppm) through a column of nonporous packing whereby separation into molecular weight (apparent size) fractions is obtained predominantly based on flow (i.e., hydrodynamic chromatography). Detection of the extremely dilute sample polymer is accomplished, e.g., by tagging the polymer with a fluorescent agent and using a flow-through fluorometer detector. The molecular weight characterization of the polymers is determined independent or less dependent of the composition of the polymer by analyzing the sample in its nonionized form.
Inventors
- 👤 Robert K. Prud'homme
- 👤 Frederick W. Stanley, Jr.
- 👤 Martin W. Langhorst
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 04:26
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/62; G01N30/74; G01N30/0005; G01N2030/001; G01N2030/022; G01N2030/027; G01N2030/621; G01N2030/625; G01N30/26; G01N30/38; G01N33/00; G01N33/44
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
180 words
A liquid chromatographic method for characterizing water soluble polymers by molecular weight and molecular weight distribution based on apparent size which comprises: (a) adding to an aqueous eluent a sample of a detectable ultra-high molecular weight polymer in a solution concentration between the detectable limit and an upper limit below the concentration at which the elution of the polymer is detrimentally influenced by concentration, the sample added being dissolved in a primarily aqueous diluent not incompatible with the eluent, the added sample volume being not greater than that volume which would detrimentally influence the chromatography; (b) passing the combined eluent and sample at a low flow rate which does not influence the elution position of the sample through a porous body composed of a packed bed of impenetrable particles whereby the apparent size fractions of the polymer sample are separated by flow chromatography; (c) detecting the amount of the eluting apparent size fractions of the polymer species; and (d) using the data of step (c) to characterize the molecular weight and molecular weight distribution of the detected water soluble polymer.
Claim 2
Dependent Claim
180 words
A liquid chromatographic method for characterizing water soluble polymers by molecular weight and molecular weight distribution based on apparent size which comprises: (a) adding to an aqueous eluent a sample of a detectable ultra-high molecular weight polymer in a solution concentration between the detectable limit and an upper limit below the concentration at which the elution of the polymer is detrimentally influenced by concentration, the sample added being dissolved in a primarily aqueous diluent not incompatible with the eluent, the added sample volume being not greater than that volume which would detrimentally influence the chromatography; (b) passing the combined eluent and sample at a low flow rate which does not influence the elution position of the sample through a porous body composed of a packed bed of impenetrable particles whereby the apparent size fractions of the polymer sample are separated by flow chromatography; (c) detecting the amount of the eluting apparent size fractions of the polymer species; and (d) using the data of step (c) to characterize the molecular weight and molecular weight distribution of the detected water soluble polymer.
Claim 3
Dependent Claim
29 words
The method of claim 1 used for characterizing the molecular weight and molecular weight distribution of polymer samples of about ≧2 million weight average molecular weight (M w ).
Claim 4
Dependent Claim
38 words
The method of claim 2 for characterizing a polyelectrolyte water soluble polymer using for the eluent, an aqueous solution the pH of which is controlled to convert or maintain the polymer of polyelectrolyte as a relatively nonionic species.
Claim 5
Dependent Claim
130 words
A liquid chromatographic method for characterizing water soluble polymers by molecular weight and molecular weight distribution based on apparent size which comprises: (a) tagging the polymer with a fluorescent group; (b) adding the polymer in aqueous diluent to an aqueous eluent; (c) passing the combined eluent and sample at a low flow rate which does not influence the elution position of the sample through a porous body composed of a packed bed of impenetrable particles whereby the apparent size fractions of the polymer sample are separated by flow chromatography; (d) detecting the amount of the eluting apparent size fractions of the polymer species based on fluorescence detection; and (e) using the data of step (d) to characterize the molecular weight and molecular weight distribution of the detected water soluble polymer.
Claim 6
Dependent Claim
130 words
A liquid chromatographic method for characterizing water soluble polymers by molecular weight and molecular weight distribution based on apparent size which comprises: (a) tagging the polymer with a fluorescent group; (b) adding the polymer in aqueous diluent to an aqueous eluent; (c) passing the combined eluent and sample at a low flow rate which does not influence the elution position of the sample through a porous body composed of a packed bed of impenetrable particles whereby the apparent size fractions of the polymer sample are separated by flow chromatography; (d) detecting the amount of the eluting apparent size fractions of the polymer species based on fluorescence detection; and (e) using the data of step (d) to characterize the molecular weight and molecular weight distribution of the detected water soluble polymer.
Claim 7
Dependent Claim
29 words
The method of claim 4 used for characterizing the molecular weight and molecular weight distribution of polymer samples of about ≧2 million weight average molecular weight (M w ).
Claim 8
Dependent Claim
37 words
The method of claim 4 for characterizing a polyelectrolyte water soluble polymer using for the eluent, an aqueous solution the pH of which is controlled to convert or maintain the polymer polyelectrolyte as a relatively nonionic species.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-12-15 | 1990-06-16 | 1990-12-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-12-15 | 1994-06-16 | 1994-12-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-12-15 | 1998-06-16 | 1998-12-16 | $7700.00 | Window Closed / Lapsed |