US 7,985,593 B2Granted

Apparatus and method for polymer characterization

AssigneeDow Global Technologies LLC

InventorsDavid T. Gillespie, Colin Li Pi Shan, Lonnie G. Hazlitt, Alexander W. DeGroot, Peter B. Arnoudse, Charles Allen Williams

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Abstract

Apparatus for GPC/TREF and TREF/GPC characterization of a polymer sample. The apparatus provides for the automated and integrated use of multiple TREF columns and a GPC system employing a multiple flow through detectors. In addition, a method for TREF/GPC characterization of a polymer sample by GPC analysis of TREF fractions at increasing TREF elution temperatures from multiple TREF columns operated in a coordinated and synchronized temperature cycle for increased sample throughput. Also, a method for GPC/TREF characterization of a polymer sample by GPC fractionation followed by TREF fractionation of the GPC fractionations.

Claims4

Dependent claims

A method for GPC/TREF characterization of a polymer sample, comprising the steps of:

(a) introducing a sample of a polymer to be characterized into a stream of eluent flowing through a gel permeation chromatography column to produce successive elution volumes from the gel permeation chromatography column wherein the polymer sample elutes therefrom substantially according to the molecular weight distribution of the polymer sample;
(b) flowing a first elution volume from the gel permeation chromatography column into a first in-line TREF column at an elevated temperature;
(c) flowing a second elution volume from the gel permeation chromatography column into a second in-line TREF column at an elevated temperature;
(d) cooling the first TREF column to precipitate polymer in the first elution volume in the first TREF column;
(e) cooling the second TREF column to precipitate polymer in the second elution volume in the second TREF column;
(f) flowing a stream solvent through the second TREF column while heating the second TREF column to dissolve the polymer precipitated therein into the flowing stream of solvent;
(g) flowing the stream of solvent from the second TREF column of step (f) through a flow through detector to detect the polymer in the stream of solvent as the polymer dissolves in the solvent as the second TREF column is heated;
(h) flowing a stream solvent through the first TREF column while heating the first TREF column to dissolve the polymer precipitated therein into the flowing stream of solvent;
(i) flowing the stream of solvent from the first TREF column of step (h) through a flow through detector of step (g) to detect the polymer in the stream of solvent as the polymer dissolves in the solvent as the first TREF column is heated.

6 more elements

Apparatus capable of being used for GPC/TREF characterization of a polymer sample or for TREF/GPC characterization of a polymer sample, the apparatus comprising:

(a) an eluent reservoir;
(b) a pump in liquid communication with the eluent reservoir;
(c) a sample injection valve in liquid communication with the pump;
(d) a two position six-port valve in liquid communication with the sample injection valve;
(e) a gel permeation chromatography column having an inlet and an outlet, the inlet being in liquid communication with the six-port valve, the outlet being in liquid communication with the six-port valve;
(f) a flow-through infrared detector in fluid communication with the six-port valve;
(g) a flow-through light scattering detector in liquid communication with the infra-red detector;
(h) a flow-through viscosity detector in liquid communication with the light scattering detector;
(i) a waste reservoir in liquid communication with the viscosity detector;
(j) a first tee in liquid communication with the six-port valve;
(k) a first on-off valve in liquid communication with the first tee;
(l) a second tee in liquid communication with the six-port valve and with the first on-off valve;
(m) a first oven containing elements (c)-(h) and (j) and (l);
(n) a two position three port valve in liquid communication with the first tee;
(o) a cross in liquid communication with the three-port valve;
(p) a first temperature equilibrium conduit in liquid communication at one end thereof with the three port valve;
(q) a second temperature equilibrium conduit in liquid communication at one end thereof with the cross and at the other end thereof with the other end of the first temperature equilibrium conduit;
(r) a third tee in liquid communication with the first cross;
(s) a fourth tee in liquid communication with the third tee;
(t) a second on-off valve in liquid communication with the fourth tee;
(u) a second oven containing elements (n), (o), and (q)-(t);
(v) a third on-off valve in liquid communication with the first cross;
(w) a fourth on-off valve in liquid communication with the third tee;
(x) a fifth on off valve in liquid communication with the fourth tee;
(y) a first TREF column having an inlet and an outlet, the inlet of the first TREF column being in liquid communication with the third on-off valve;
(z) a second TREF column having an inlet and an outlet, the inlet of the second TREF column being in liquid communication with the fourth on-off valve;
(a′) a third TREF column having an inlet and an outlet, the inlet of the third TREF column being in liquid communication with the fifth on-off valve;
(b′) a fifth tee in liquid communication with the outlet of the first TREF column and with the second tee;
(c′) a sixth tee in liquid communication with the outlet of the second TREF column and with the fifth tee;
(d′) a seventh tee in liquid communication with the outlet of the third TREF column and the second on-off valve as well as the sixth tee;
(e′) a third oven containing elements (v) and (y);
(f′) a fourth oven for containing elements (w) and (z′);
(g′) a fifth oven for containing elements (x) and (a′);
(h′) a sixth oven for containing elements (b′), (c′) and (d′);
and (I′) a seventh oven for containing a portion of the liquid connection between (t) and (d′).

32 more elements

Dependencies are inferred from the claim text.

Facts

Application: 11/794,417Filed 19 Jan 2006 · us provisional application
Priority: 24 Jan 2005
Published: US 2008/0166817 A110 Jul 2008
Granted: 26 Jul 2011
Term ends: Not estimatedThe source records don’t support an estimate.

Classification8 codes

G01N 30/468
Using more than one column: involving switching between different column configurations
G01N 25/147
By using distillation, extraction, sublimation, condensation, freezing, or crystallisation: by cristallisation
G01N 30/463
With serial coupling of separation columns: for multidimensional chromatography
G01N 30/54
Physical parameters: temperature