Overlaid injection for rapid characterizations of polymers

• US 6,454,947 B1
• Filed: 11/28/2000
• Issued: 09/24/2002
• Est. Priority Date: 04/03/1998
• Status: Expired due to Term

• Current Assignee: Intermolecular Incorporated
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Carlson, Eric, Petro, Miroslav, Safir, Adam, Nielsen, Ralph B.
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US09/728,375
• Time in Patent Office: 665 Days
• Field of Search: 210/143, 210/198.2, 210/634, 210/635, 210/656, 210/659, 210/745, 422/63, 422/69, 422/70, 422/81, 422/82.05, 422/100, 436/179, 436/180, 436/164, 436/161, 73/615.2, 73/615.5, 73/615.6, 356/337, 356/338, 356/339
• US Class Current: 506/12
• CPC Class Codes: B01D 15/08 Selective adsorption, e.g. chromatography
• CPC Class Codes: B01D 15/14 relating to the introduction of the feed to the apparatus
• CPC Class Codes: B01D 15/1871 placed in series
• CPC Class Codes: B01D 15/1885 placed in parallel
• CPC Class Codes: B01D 15/34 Size selective separation, e.g. size exclusion chromatography, gel filtration, permeation
• CPC Class Codes: B01J 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
• CPC Class Codes: B01J 19/26 Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• CPC Class Codes: B01J 2219/00274 Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/00587 High throughput processes
• CPC Class Codes: B01J 2219/00707 separated from the reactor apparatus
• CPC Class Codes: B01J 2219/00722 Nucleotides
• CPC Class Codes: C40B 40/14 Libraries containing macromolecular compounds and not covered by groups C40B40/06 - C40B40/12
• CPC Class Codes: G01N 15/0205 by optical means
• CPC Class Codes: G01N 2015/0288 Sorting the particles
• CPC Class Codes: G01N 2015/0294 Particle shape
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 30/02 Column chromatography
• CPC Class Codes: G01N 30/16 Injection G01N30/24 takes precedence
• CPC Class Codes: G01N 30/24 Automatic injection systems
• CPC Class Codes: G01N 30/30 : of temperature
• CPC Class Codes: G01N 30/461 : with serial coupling of separation columns
• CPC Class Codes: G01N 30/466 : with separation columns in parallel
• CPC Class Codes: G01N 30/54 : Temperature
• CPC Class Codes: G01N 30/6052 : body
• CPC Class Codes: G01N 30/88 : Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
• CPC Class Codes: G01N 33/44 : Resins; rubber; leather
• CPC Class Codes: G01N 35/085 : Flow Injection Analysis
• CPC Class Codes: G01N 35/1097 : characterised by the valves valves in general F16K
• CPC Class Codes: Y10T 436/25 : including sample preparation

Abstract

A method is disclosed for characterizing a plurality of non-biological polymer samples. The method includes the steps of injecting a first non-biological polymer sample into a mobile-phase of a liquid chromatography system, chromatographically separating at least one sample component of the injected first sample from other sample components thereof in a chromatographic column, detecting at least one property of the separated sample component of the first sample, injecting a second non-biological polymer sample into the mobile-phase of the liquid chromatography system while advancing the first sample to the chromatographic column, chromatographically separating at least one sample component of the injected second sample from other sample components thereof, and detecting at least one property of the separated sample component of the second sample.

Claims

1. A method for characterizing a plurality of non-biological polymer samples, the method comprising

(a) injecting a first non-biological polymer sample into a mobile-phase of a liquid chromatography system,

(b) chromatographically separating at least one sample component of the injected first sample from other sample components thereof in a chromatographic column,

(c) detecting at least one property of the separated sample component of the first sample,

(d) injecting a second non-biological polymer sample into the mobile-phase of the liquid chromatography system while advancing the first sample to the chromatographic column,

(e) chromatographically separating at least one sample component of the injected second sample from other sample components thereof, and

(f) detecting at least one property of the separated sample component of the second sample.

4. The method of claims 1, 2 or 3 further comprising repeating steps (a) through (f) to detect a property of at least eight different polymer samples or of a component thereof.

5. The method of claims 1 or 3 wherein at least one component from the first sample and at least one component from the second sample simultaneously reside in a detection cavity of the detector.

6. The method of claims 1, 2 or 3 wherein the property of the separated sample components is detected with an evaporative light-scattering detector.

7. The method of claims 1, 2 or 3 wherein the weight-average molecular weight of the separated sample components is determined based on a property detected with a detector insensitive to sample components having a weight-average molecular weight of less than about 1000.

8. The method of claims 1, 2 or 3 wherein the weight-average molecular weight of the separated sample components is determined based on the scattered light detected with an evaporative light-scattering detector.

10. The method of claims 1, 2 or 3 wherein the separation medium comprises stationary-phase media for size exclusion chromatography.

11. The method of claims 1, 2 or 3 wherein the separation medium comprises porous, stationary phase media for gel permeation chromatography.

12. The method of claims 1, 2 or 3 wherein the chromatographic column defines a separation cavity having an aspect ratio ranging from about 0.1 to about 1.

2. A method for characterizing a plurality of non-biological polymer samples, the method comprising

(a) injecting a first non-biological polymer sample into a mobile-phase of a liquid chromatography system,

(b) chromatographically separating at least one sample component of the injected first sample from other sample components thereof in a chromatographic column,

(c) detecting at least one property of the separated sample component of the first sample,

(d) injecting a second non-biological polymer sample into the mobile-phase of the liquid chromatography system,

(e) chromatographically separating at least one sample component of the injected second sample from other sample components thereof, and

(f) detecting at least one property of the separated sample component of the second sample,

the second polymer sample being injected into the mobile phase such that at least one component from the first sample and at least one component from the second sample simultaneously reside in a detection cavity of the detector.

3. A method for characterizing a plurality of non-biological polymer samples, the method comprising

(a) injecting a first non-biological polymer sample into a mobile-phase of a liquid chromatography system,

(b) chromatographically separating at least one sample component of the injected first sample from other sample components thereof in a chromatographic column,

(c) detecting at least one property of the separated sample component of the first sample,

(d) injecting a second non-biological polymer sample into the mobile-phase of the liquid chromatography system while (i) advancing the first sample to the chromatographic column, while (ii) separating at least one sample component of the injected first sample from other sample components thereof, or while (iii) detecting at least one property of the separated sample component of the first sample,

(e) chromatographically separating at least one sample component of the injected second sample from other sample components thereof, and

(f) detecting at least one property of the separated sample component of the second sample,

each of the first and second polymer samples being members of a library of polymerization product mixtures.

9. The method of claim 3 wherein the library of polymerization product mixtures are simultaneously synthesized in a parallel polymerization reactor.