# US 5,707,587 A · Apparatus for in situ, non-invasive polymer cure determination

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 5,707,587 A
- Document ID: US5707587A
- Status: Granted
- Kind: A
- Application number: 08/752,830
- Filed: 1996-11-20
- Granted: 1998-01-13
- Earliest claimed: 1995-04-24
- Assignees: Board of Trustees operating Michigan State University
- Inventors: Gary J. Blanchard; Julie L. Jessop; Alec B. Scranton
- Web page: https://patentgrep.com/patent/US5707587A

## CPC

- G01N 21/643: {non-biological material}
- B29C 35/0288: {Controlling heating or curing of polymers during moulding, e.g. by measuring temperatures or properties of the polymer and regulating the process (controlling or regulating chemical, physical or physico- chemical processes in general B01J19/0006)}
- C08J 3/248: {Measuring crosslinking reactions}
- G01N 33/44: Resins; Plastics; Rubber; Leather
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)

## Abstract

A method and apparatus (10) for detection of the degree of cure of a polymer in situ and non-invasively. The method and apparatus uses a solvatochromic probe molecule which upon curing produces a shift in the fluorescence emission spectrum as compared to a liquid polymerizable composition. The method and apparatus is particularly adapted for poly(vinyl) polymers. Preferred solvatochromic probe molecules are oxazones and pyrene.

## Claims

### Claim 1

An apparatus for determining an extent of curing of a cured polymer which comprises:
(a) a detection means which measures a shift in fluorescence emission spectrum during polymerization of a liquid polymerizable composition to the cured polymer from a solvatochromic probe molecule, which is a polycyclic aromatic compound in an amount up to about 10.sup.-3 weight percent of the polymerizable composition, wherein the probe molecule has a first fluorescence emission spectrum in the liquid polymerizable composition and a shifted second fluorescence emission spectrum in the cured polymer, wherein the detection means includes a probe means mounted adjacent to the polymer for detecting the fluorescence;
(b) a light source which can be directed at the polymerizable composition so that the fluorescence emission spectrum produced by the probe molecule is detected by the probe means;
(c) a support for the fluid polymer during the curing to the cured polymer; and
(d) calculating means for calculating at a given wavelength a ratio of the second fluorescence emission spectrum and the first fluorescence emission spectrum at least for the liquid polymerizable composition and during the polymerization to the cured polymer so that the extent of curing can be determined, and wherein the shift in the fluorescence is detected beyond a gel point of the polymer.

### Claim 2 (depends on 1)

The apparatus of claim 1 wherein the detection means and calculating means are operable at pre-selected intervals of time during the curing.

### Claim 3 (depends on 1)

The apparatus of claim 1 wherein the light source is a laser.

### Claim 4 (depends on 1)

The apparatus of claim 1 wherein the probe means is connected to an optical cable so that the light from the light source is directed at the reaction mixture.