# US 10,309,901 B2 · Water-sensitive fluorophores for moisture content evaluation in hygroscopic polymers

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- Number: US 10,309,901 B2
- Document ID: US10309901B2
- Status: Granted
- Kind: B2
- Application number: 15/436,376
- Filed: 2017-02-17
- Published: 2018-08-23
- Granted: 2019-06-04
- Earliest claimed: 2017-02-17
- Assignees: International Business Machines Corporation
- Applicants: International Business Machines Corporation
- Inventors: Eric J. Campbell; Sarah K. Czaplewski; Joseph Kuczynski; Timothy J. Tofil
- Web page: https://patentgrep.com/patent/US10309901B2

## CPC

- G01N 21/643: {non-biological material}
- G01N 21/81: Indicating humidity
- G01N 33/18: Water
- G01N 33/442: {Resins; Plastics}
- G01N 21/274: {Calibration, base line adjustment, drift correction}
- G01N 2021/6443: {Fluorimetric titration}
- G01N 2021/7786: {Fluorescence}
- 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)

## Abstract

A process of utilizing a water-sensitive fluorophore for moisture content evaluation in a hygroscopic polymer includes forming a blend that includes a hygroscopic polymer resin and a water-sensitive fluorophore. The process includes forming pellets having a particular geometry from the blend, determining fluorescence properties of at least one of the pellets, and determining moisture content of at least one of the pellets. The process also includes generating a calibration curve for the particular pellet geometry by correlating the fluorescence properties with the moisture content. The process further includes providing the calibration curve for non-destructive moisture content evaluation of a material derived from the pellets.

## Claims

### Claim 1

A process of utilizing a water-sensitive fluorophore for moisture content evaluation in a hygroscopic polymer, the process comprising:
forming a blend that includes a hygroscopic polymer resin and a water-sensitive fluorophore;
forming pellets having a particular geometry from the blend;
determining fluorescence properties of at least one of the pellets;
determining moisture content of at least one of the pellets;
generating a calibration curve for the particular pellet geometry by correlating the fluorescence properties with the moisture content; and
providing the calibration curve for non-destructive moisture content evaluation of a material derived from the pellets.

### Claim 2 (depends on 1)

The process of claim 1, wherein the calibration curve is provided to a part manufacturing entity for moisture content evaluation after forming dried pellets by removing moisture from the pellets prior to forming an article of manufacture from the dried pellets.

### Claim 3 (depends on 2)

The process of claim 2, wherein the article of manufacture is formed by injection molding.

### Claim 4 (depends on 2)

The process of claim 2, wherein the part manufacturing entity measures fluorescence properties of the dried pellets and utilizes the calibration curve to determine a moisture content level of the dried pellets based on the measured fluorescence properties of the dried pellets.

### Claim 5 (depends on 4)

The process of claim 4, further comprising forming the article of manufacture from the dried pellets when the moisture content level of the dried pellets is a satisfactory moisture level.

### Claim 6 (depends on 4)

The process of claim 4, further comprising performing an additional drying operation to remove additional moisture from the dried pellets when the moisture content level of the dried pellets is an unsatisfactory moisture level.

### Claim 7 (depends on 1)

The process of claim 1, wherein the hygroscopic polymer resin includes a nylon resin.

### Claim 8 (depends on 1)

The process of claim 1, wherein the hygroscopic polymer resin includes an acrylonitrile butadiene styrene (ABS) resin, an acrylic resin, a polyurethane resin, a polyethylene terephthalate (PET) resin, or a polybutylene terephthalate (PBT) resin.

### Claim 9 (depends on 1)

The process of claim 1, wherein the water-sensitive fluorophore includes 5-(dimethylamino)naphthalene-1-sulfonic acid (DNSA), 5-(dimethylamino)naphthalene-1-sulfonamide (DNSM), 8-(anilino)naphthalene-1-sulfonic acid (ANSA), or a combination thereof.

### Claim 10 (depends on 1)

The process of claim 1, wherein the moisture content of at least one of the pellets is determined by Karl Fischer titration.

### Claim 11

A process of utilizing a water-sensitive fluorophore for moisture content evaluation in a hygroscopic polymer, the process comprising:
receiving, from a pellet manufacturing entity, pellets that are formed from a blend that includes a hygroscopic polymer resin and a water-sensitive fluorophore;
receiving, from the pellet manufacturing entity, a calibration curve that correlates fluorescence properties of the pellets with moisture content of the pellets;
forming dried pellets by removing moisture from the pellets prior to forming an article of manufacture from the dried pellets;
measuring fluorescence properties of the dried pellets;
utilizing the calibration curve to determine a moisture content level of the dried pellets based on the measured fluorescence properties of the dried pellets; and
determining whether to form the article of manufacture from the dried pellets based on whether the moisture content level of the dried pellets corresponds to a satisfactory moisture level.

### Claim 12 (depends on 11)

The process of claim 11, further comprising performing an additional drying operation to remove additional moisture from the dried pellets when the moisture content level of the dried pellets corresponds to an unsatisfactory moisture level.

### Claim 13 (depends on 11)

The process of claim 11, further comprising forming the article of manufacture from the dried pellets when the moisture content level of the dried pellets corresponds to the satisfactory moisture level, the article of manufacture having a particular part geometry.

### Claim 14 (depends on 13)

The process of claim 13, further comprising performing one or more moisture conditioning operations on the article of manufacture, allowing the article of manufacture to reach an equilibrium moisture content, or a combination thereof.

### Claim 15 (depends on 14)

The process of claim 14, further comprising:
determining fluorescence properties of the article of manufacture;
determining moisture content of the article of manufacture; and
generating a part-specific calibration curve for the particular part geometry by correlating the fluorescence properties of the article of manufacture with the moisture content of the article of manufacture.

### Claim 16 (depends on 15)

The process of claim 15, further comprising providing the part-specific calibration curve to a part monitoring entity for non-destructive moisture content evaluation of the article of the manufacture in a deployment environment.

### Claim 17 (depends on 16)

The process of claim 16, wherein the part monitoring entity measures fluorescence properties of the article of manufacture in the deployment environment and utilizes the part-specific calibration curve to determine a moisture content level of the article of manufacture based on the measured fluorescence properties of the article of manufacture in the deployment environment.

### Claim 18

A process of utilizing a water-sensitive fluorophore for moisture content evaluation in a hygroscopic polymer, the process comprising:
measuring fluorescence properties of an article of manufacture that is deployed to a deployment environment, wherein the article of manufacture is manufactured from pellets that are formed from a blend that includes a hygroscopic polymer resin and a water-sensitive fluorophore;
receiving a part-specific calibration curve that correlates fluorescence properties of the article of manufacture with moisture content of the article of manufacture;
utilizing the part-specific calibration curve to determine a moisture content level of the article of manufacture based on the measured fluorescence properties of the article of manufacture; and
determining whether to perform a corrective action based on whether the moisture content level of the article of manufacture corresponds to a satisfactory moisture level.

### Claim 19 (depends on 18)

The process of claim 18, wherein the corrective action includes removal of the article of manufacture from the deployment environment.

### Claim 20 (depends on 18)

The process of claim 18, wherein the environmental conditions associated with the deployment environment correspond to a high temperature environment, a low humidity environment, or a combination thereof, and wherein the environmental conditions are associated with a high probability of the article of manufacture becoming brittle as a result of moisture removal.
