US5650722A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Using resin age factor to obtain measurements of improved accuracy of one or more polymer properties with an on-line NMR system
Assignee: Progression Inc
•
Filing: 1996-05-07
•
Granted: 1997-07-22
•
Expires: 2016-05-07
Abstract
Abstract A real-time, on-line nuclear magnetic resonance (NMR) system, and related method, can predict various properties of interest of a sample of polymer material. A regression or neural network technique is used to develop a model based upon manipulated NMR output and a resin age factor which compensates for time dependent aging phenomena and enhance predictive accuracy of the model. In a preferred embodiment, the resin age factor is a function of elapsed cycle time prior to sample measurement, sample temperature at time of measurement, and/or sample form. The polymer can be a plastic such as polyethylene, polypropylene, or polystyrene, or a rubber such as ethylene propylene rubber.
Inventors
- 👤 Thomas B. Smith
- 👤 Ajoy K. Roy
- 👤 Christian I. Tanzer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 12:31
CPC Classifications
G; G01; G01R; G01R33/00; G01R33/20; G01R33/44; G01R33/46; G01R33/4625; G01N; G01N24/00; G01N24/08; G01N24/085; G01R33/28; G01R33/38; G01R33/389; G01N24/082
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
223 words
A method for predicting a value of a property of a polymer sample in real time from an on-line production process, said method comprising: storing a model useful for predicting a value of a property of interest of a production polymer sample, said model generated by: a) acquiring free induction decay curves for polymer samples having known values of said property of interest; b) applying an iterative technique to derive respective component curve equations from each of said free induction decay curves; c) calculating respective component curve equation constants; d) acquiring process data for said known samples; and e) generating said model using said constants, said process data, and said known values; providing a production sample having an unknown value of said property of interest; applying a base magnetic field to the production sample to effect precession of nuclei of the production sample; modifying the precession; receiving a resulting relaxation signal representative of a free induction decay of nuclei of the production sample; digitizing said relaxation signal; applying an iterative technique to derive respective component curve equations from said relaxation signal; calculating respective component curve equation constants; acquiring process data for said production sample; and applying said constants and said process data to said model to predict the value of the property of interest, wherein said process data comprises a resin age factor.
Claim 2
Independent Claim
223 words
A method for predicting a value of a property of a polymer sample in real time from an on-line production process, said method comprising: storing a model useful for predicting a value of a property of interest of a production polymer sample, said model generated by: a) acquiring free induction decay curves for polymer samples having known values of said property of interest; b) applying an iterative technique to derive respective component curve equations from each of said free induction decay curves; c) calculating respective component curve equation constants; d) acquiring process data for said known samples; and e) generating said model using said constants, said process data, and said known values; providing a production sample having an unknown value of said property of interest; applying a base magnetic field to the production sample to effect precession of nuclei of the production sample; modifying the precession; receiving a resulting relaxation signal representative of a free induction decay of nuclei of the production sample; digitizing said relaxation signal; applying an iterative technique to derive respective component curve equations from said relaxation signal; calculating respective component curve equation constants; acquiring process data for said production sample; and applying said constants and said process data to said model to predict the value of the property of interest, wherein said process data comprises a resin age factor.
Claim 3
Dependent Claim
31 words
The method of claim 1 wherein said resin age factor is a function of at least one parameter selected from the group consisting of cycle time, sample temperature, and sample form.
Claim 4
Dependent Claim
28 words
The method of claim 2 wherein said cycle time comprises time lapse between about the step of providing a production sample and the step of modifying the precession.
Claim 5
Dependent Claim
22 words
The method of claim 2 wherein said sample temperature comprises temperature of a sample at about the step of modifying the precession.
Claim 6
Dependent Claim
21 words
The method of claim 2 wherein said sample form is selected from the group consisting of powder form and pellet form.
Claim 7
Dependent Claim
35 words
The method of claim 1 wherein said iterative technique applied to either of said free induction decay curve or said relaxation signal is selected from the group consisting of Marquardt-Levenberg, Gauss-Jordan, Newton-Raphson, and steepest descent.
Claim 8
Dependent Claim
23 words
The method of claim 1 wherein said component curve equations are selected from the group consisting of Abragam, Gaussian, and exponential curve equations.
Claim 9
Dependent Claim
28 words
The method of claim 1 wherein said component curve equation constants are selected from the group consisting of ratios, squares, cross products of Y-axis intercepts, and decay times.
Claim 10
Dependent Claim
31 words
The method of claim 1 wherein said property of interest is selected from the group consisting of xylene solubles, density, rubber/oil content, melt index, flow rate ratio, melt flow, and crystallinity.
Claim 11
Dependent Claim
22 words
The method of claim 1 wherein said production polymer sample is selected from the group consisting of rubber, polypropylene, polyethylene, and polystyrene.
Claim 12
Dependent Claim
33 words
The method of claim 1 wherein said model generating substep (e) is accomplished by a technique selected from the group consisting of principal component regression, partial least square regression, and neural network techniques.
Claim 13
Dependent Claim
246 words
Apparatus for predicting a value of a property of a polymer sample in real time from an on-line production process, said apparatus comprising: means for storing a model useful for predicting a value of a property of interest of a production polymer sample; means for generating said model comprising means for: a) acquiring free induction decay curves for polymer samples having known values of said property of interest, b) applying an iterative technique to derive respective component curve equations from each of said free induction decay curves, c) calculating respective component curve equation constants, d) acquiring process data for said known samples, and e) generating said model using said constants, said process data, and said known values; means for providing a production sample having an unknown value of said property of interest; means for applying a base magnetic field to the production sample to effect precession of nuclei of the production sample; means for modifying the precession; means for receiving a resulting relaxation signal representative of a free induction decay of nuclei of the production sample; means for digitizing said relaxation signal; means for applying an iterative technique to derive respective component curve equations from said relaxation signal; means for calculating respective component curve equation constants; means for acquiring process data for said production sample; and means for applying said constants and said process data to said model to predict the value of the property of interest, wherein said process data comprises a resin age factor.
Claim 14
Dependent Claim
246 words
Apparatus for predicting a value of a property of a polymer sample in real time from an on-line production process, said apparatus comprising: means for storing a model useful for predicting a value of a property of interest of a production polymer sample; means for generating said model comprising means for: a) acquiring free induction decay curves for polymer samples having known values of said property of interest, b) applying an iterative technique to derive respective component curve equations from each of said free induction decay curves, c) calculating respective component curve equation constants, d) acquiring process data for said known samples, and e) generating said model using said constants, said process data, and said known values; means for providing a production sample having an unknown value of said property of interest; means for applying a base magnetic field to the production sample to effect precession of nuclei of the production sample; means for modifying the precession; means for receiving a resulting relaxation signal representative of a free induction decay of nuclei of the production sample; means for digitizing said relaxation signal; means for applying an iterative technique to derive respective component curve equations from said relaxation signal; means for calculating respective component curve equation constants; means for acquiring process data for said production sample; and means for applying said constants and said process data to said model to predict the value of the property of interest, wherein said process data comprises a resin age factor.
Claim 15
Dependent Claim
31 words
The apparatus of claim 12 wherein said resin age factor is a function of at least one parameter selected from the group consisting of cycle time, sample temperature, and sample form.
Claim 16
Dependent Claim
26 words
The apparatus of claim 13 wherein said cycle time comprises time lapse between about when the production sample is provided and when the precession is modified.
Claim 17
Dependent Claim
22 words
The apparatus of claim 13 wherein said sample temperature comprises temperature of a sample at about the time the precession is modified.
Claim 18
Dependent Claim
21 words
The apparatus of claim 13 wherein said sample form is selected from the group consisting of powder form and pellet form.
Claim 19
Dependent Claim
35 words
The apparatus of claim 12 wherein said iterative technique applied to either of said free induction decay curve or said relaxation signal is selected from the group consisting of Marquardt-Levenberg, Gauss-Jordan, Newton-Raphson, and steepest descent.
Claim 20
Dependent Claim
23 words
The apparatus of claim 12 wherein said component curve equations are selected from the group consisting of Abragain, Gaussian, and exponential curve equations.
Claim 21
Dependent Claim
28 words
The apparatus of claim 12 wherein said component curve equation constants are selected from the group consisting of ratios, squares, cross products of Y-axis intercepts, and decay times.
Claim 22
Dependent Claim
31 words
The apparatus of claim 12 wherein said property of interest is selected from the group consisting of xylene solubles, density, rubber/oil content, melt index, flow rate ratio, melt flow, and crystallinity.
Claim 23
Dependent Claim
22 words
The apparatus of claim 12 wherein said production polymer sample is selected from the group consisting of rubber, polypropylene, polyethylene, and polystyrene.
Claim 24
Dependent Claim
32 words
The apparatus of claim 12 wherein said means for generating said model utilizes a technique selected from the group consisting of principal component regression, partial least square regression, and neural network techniques.
References Cited (Backward Citations)
US5049819A
Cited
WO1992016851A1
Cited
US5015954A
Cited
US5519319A
Cited
WO1993010468A1
Cited
US5302896A
Cited
US5162103A
Cited
US5302897A
Cited
WO1994009379A1
Cited
US5319308A
Cited
WO1994009380A1
Cited
US5367260A
Cited
WO1995006882A1
Cited
US5408181A
Cited
WO1995008777A1
Cited
WO1995008776A1
Cited
US5420508A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 2000-07-21 | 2001-01-20 | 2001-07-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2004-07-21 | 2005-01-20 | 2005-07-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2008-07-21 | 2009-01-20 | 2009-07-22 | $7700.00 | Window Closed / Lapsed |