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High-temperature characterization of polymers with HPLC system having multiple mobile-phase reservoirs

a polymerization and high-temperature technology, applied in the field of polymer characterization, can solve problems such as the influence of calibration standards and methods on the overall system speed, and achieve the effect of preventing a backlog of uncharacterized polymerization product samples and achieving higher characterization throughputs

Inactive Publication Date: 2001-11-08
INTERMOLECULAR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0013] It is therefore an object of the present invention to provide systems and protocols for characterizing combinatorial libraries of polymer samples, and particularly, libraries of or derived from polymerization product mixtures, to facilitate the discovery of commercially important polymeric materials, catalysts, polymerization conditions and / or post-synthesis processing conditions. It is also an object of the invention to provide polymer characterization systems and protocols that can be employed in near-real-time industrial process control.

Problems solved by technology

In addition, rapid, indirect calibration standards and methods impact overall system speed.

Method used

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  • High-temperature characterization of polymers with HPLC system having multiple mobile-phase reservoirs
  • High-temperature characterization of polymers with HPLC system having multiple mobile-phase reservoirs
  • High-temperature characterization of polymers with HPLC system having multiple mobile-phase reservoirs

Examples

Experimental program
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Effect test

example 1

Auto-sampling with Single Robotic Arm

[0292] This example demonstrates rapid, automated (robotic) preparation and sampling of polymer libraries using one robotic arm.

[0293] Conventional, Commercially-available Auto-sampler

[0294] A conventional, commercially-available auto-sampler was evaluated. A Gilson.RTM., (Middleton, Wis.) Model 215 is described by Gilson.RTM. as a computer-controlled XYZ robot with stationary rack. It was mounted with a steel needle probe, a syringe pump, and a valve and sample loop connected to an HPLC system. This auto-sampler, as programmed by Gilson.RTM., required slightly more than 90 seconds to perform the following sequence of operations: (1)drawing 100 .mu.L water from position 1 of a microtiter plate; (2) loading a 50 .mu.L sample loop with the water; (3) actuating the injection valve to inject the sample into the flow system; (4) cleaning the probe needle by flushing in preparation for the next sample; and (5) repeating steps (1) through (4) with water...

example 2

Auto-sampler with Two Robotic Arms

[0301] This example demonstrates rapid, automated (robotic) preparation and sampling of combinatorial libraries using two robotic arms, allowing for multiple, simultaneous analyses.

[0302] A robotic sampler was prepared in a similar manner to Example 1, except using a two-arm XYZ robot (Cavro, model RSP 9652), two injection valves (Valco, model EHC8W), and four pumps (Cavro, model XL 3000). For each arm, two pumps were connected in series to a single probe needle on the arm, one pump fitted with a 500 .mu.L syringe, and one pump with a 5000 .mu.L syringe. In this configuration, good flow precision was obtained with the smaller volume pump when needed, while the larger volume pump can deliver instantaneous flow rates of approximately 300 mL / min and overall flow rates greater than 100 mL / min, allowing for very rapid rinsing, washing, and sample manipulation.

[0303] Liquid samples from an array of vessels were rapidly loaded and injected using this syste...

example 3

Precipitation--Redissolution Chromatography

[0304] This example demonstrates the use of a liquid chromatography system for rapid chromatographic separation of polystyrene polymer standards using precipitation-redissolution chromatography with a mobile-phase composition gradient. The results provided a calibration for the chromatographic system and conditions.

[0305] The robotic auto-sampler and injection valve set-up as in Example 1 was fitted with two sample loops (each having 50 microliter volume) in combination with a high-pressure liquid chromatographic (HPLC) apparatus comprising a two-pump gradient chromatography system, primed with methanol and tetrahydrofuran (THF) solvent. A porous crosslinked polystyrene monolithic column was utilized, prepared as described in Frechet et al., Journal of Chromatography A, 752 (1996) 59-66 and Frchet et al., Anal. Chem. 1996, 68, 315-321. The HPLC system was configured such that the combined flow of the pump system passed through the valve, th...

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Abstract

Rapid characterization and screening of polymer samples to determine average molecular weight, molecular weight distribution and other properties is disclosed. Rapid flow characterization systems and methods, including liquid chromatography and flow-injection analysis systems and methods are preferably employed. High throughput, automated sampling systems and methods, high-temperature characterization systems and methods, and rapid, indirect calibration compositions and methods are also disclosed. The described methods, systems, and devices have primary applications in combinatorial polymer research and in industrial process control.

Description

[0001] This application claims priority under 35 U.S.C. Sec. 119(e) to U.S. Provisional Application Ser. No. 60 / 080,652, filed Apr. 3, 1998 by Safir et al., which is hereby incorporated by reference for all purposes.[0002] This application is related to the following U.S. patent applications filed on the date even herewith, each of which is hereby incorporated by reference for all purposes: Ser. No. ______, entitled "Automated Sampling Methods for Rapid Characterization of Polymers", filed Apr. 2, 1999 by Petro et al. under Attorney Docket No. 99-10; Ser. No. ______, entitled "Rapid Characterization of Polymers", filed Apr. 2, 1999 by Safir et al. under Attorney Docket No. 99-9; Ser. No. ______, entitled "Flow-Injection Analysis and Variable-Flow Light Scattering Apparatus and Methods for Characterizing Polymers", filed Apr. 2, 1999 by Nielsen et al. under Attorney Docket No. 99-12; and Ser. No. ______, entitled "Indirect Calibration of Polymer Characterization Systems", filed Apr. ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01D15/08B01D15/26B01D15/32B01D15/34B01J19/00B01J19/26C40B40/14G01N1/00G01N15/02G01N30/02G01N30/16G01N30/24G01N30/30G01N30/32G01N30/46G01N30/54G01N30/60G01N30/88G01N33/44G01N35/02G01N35/08
CPCB01D15/08B01D15/14B01D15/161B01D15/26B01D15/265B01D15/325B01D15/34B01J19/0046B01J19/26B01J2219/00274B01J2219/00585B01J2219/00587B01J2219/00707B01J2219/00722C40B40/14G01N15/0205G01N30/02G01N30/16G01N30/24G01N30/30G01N30/461G01N30/466G01N30/54G01N30/6052G01N30/88G01N33/44G01N33/442G01N35/028G01N35/085G01N35/1097G01N2015/0288G01N2015/0294G01N2030/324G01N2030/885Y10S210/13
Inventor PETRO, MIROSLAVCARLSON, ERICSAFIR, ADAMNIELSEN, RALPH
Owner INTERMOLECULAR
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