Apparatus for measuring moisture of solid sample, method for measuring moisture content of solid sample, and method for analyzing imidization ratio

Patent metadata

Field	Value
Publication number	US-10928301-B2
Application number	US-201715775626-A
Country	US
Kind code	B2
Filing date	Apr 27, 2017
Priority date	Apr 27, 2016
Publication date	Feb 23, 2021
Grant date	Feb 23, 2021

Abstract

The present invention relates to an apparatus for measuring moisture of a solid sample, a method for measuring a moisture content of the solid sample, and a method for analyzing an imidization rate, and more particularly, to an apparatus for measuring moisture of a solid sample, a method for measuring a moisture content of the solid sample, and a method for analyzing an imidization rate, which detect the moisture content of the solid sample at a specific temperature by using a Karl-Fischer device capable of selectively detecting only the moisture content of the solid sample in the method for analyzing an imidization rate of the solid sample and calculate the imidization rate of the solid sample by using the detected moisture content.

First claim

The invention claimed is:

1. An apparatus for measuring moisture of a solid sample, the apparatus comprising:
an introduction unit into which the solid sample is capable of being introduced;
a furnace unit to which the solid sample is capable of being fixed, the furnace unit comprising a moisture transport pipe for supplying a moisture transport gas into the furnace unit, the furnace unit for heating and cooling the solid sample;
a control unit for controlling a threshold temperature of the furnace unit; an O-ring unit sealed between the introduction unit and the furnace unit;
a three-way valve connected to the furnace unit via the moisture transport pipe, the three-way valve for receiving and controlling moisture evaporated from the solid sample, the moisture transport gas for transporting the moisture evaporated from the solid sample to the three-way valve; and
a Karl-Fischer unit connected to the three-way valve via a metering transport pipe, the Karl-Fischer unit for measuring a detected moisture content of the solid sample from the moisture evaporated form the solid sample,
wherein the O-ring unit includes an O-ring cooling unit positioned adjacent to the O-ring unit, the O-ring cooling unit for cooling the O-ring unit,
wherein the threshold temperature of the furnace unit can be set to at least one temperature selected from the group consisting of a first threshold temperature, a second threshold temperature, and a third threshold temperature,
wherein the control unit controls the three-way valve to allow a purge of moisture from the furnace unit to outside the apparatus and to prevent transport of moisture from the furnace unit to the Karl-Fischer unit when the furnace unit is heated up to the first threshold temperature or heated up to the third threshold temperature or higher, and
wherein the control unit controls the three-way valve to prevent a purge moisture from the furnace unit to outside the apparatus and to permit transport of moisture from the furnace unit to the Karl-Fischer unit when the furnace unit is heated up to the second threshold temperature and the third threshold temperature.

2. The apparatus of claim 1 , wherein the furnace unit comprises:
a body for fixing the solid sample,
a heating unit positioned outside the body, the heating unit for heating the body, and a cooling unit positioned outside the body, the cooling unit for cooling the body.

3. The apparatus of claim 2 , wherein the cooling unit and the O-ring cooling unit use at least one of a water cooling type and an air cooling type for cooling the body and the O-ring, respectively.

4. The apparatus of claim 1 , wherein the moisture transportation gas pipe includes a moisture trap unit to remove moisture in the moisture transport gas.

5. The apparatus of claim 1 , wherein the three-way valve comprises:
a moisture transport port for receiving the moisture from the furnace unit,
a purge port for purging the moisture from the furnace unit outside of the apparatus, and
a metering port for transporting the moisture from the furnace unit to the Karl-Fischer unit.

6. The apparatus of claim 5 , wherein the control unit controls the threshold temperature of the furnace unit by controlling the heating unit and the cooling unit and by controlling the three-way valve.

7. The apparatus of claim 6 , wherein the control unit
heats or cools the furnace unit by setting a temperature of the heating unit to the first threshold temperature, then heating to the second threshold temperature, then heating to the third threshold temperature, and
then cools the furnace unit back to the first threshold temperature.

8. The apparatus of claim 7 , wherein the control unit
controls the purge port to be on and the metering port to be off when the furnace unit is heated up to the first threshold temperature or heated up to the third threshold temperature or higher, and
controls the purge port to be off and the metering port to be on when the furnace unit is heated up to the second threshold temperature and the third threshold temperature.

9. A method for analyzing a solid sample,
comprising: fixing the solid sample to a body of a furnace unit of an apparatus;
heating the body to heat the solid sample;
transporting moisture evaporated from the solid sample through a three-way valve of the apparatus, wherein the three-way valve includes a purge port for purging the moisture to outside of the apparatus, and a metering port for transporting the moisture to a Karl-Fischer unit of the apparatus;
measuring a detected moisture content of the solid sample through the moisture transported to the Karl-Fischer unit; and
cooling the body,
wherein during cooling of the body, an O-ring unit positioned between an introduction unit and the body is cooled, wherein the introduction unit is a unit of the apparatus for introducing the solid sample into the body,
wherein transporting moisture evaporated from the solid sample further comprises:
transporting the evaporated moisture to outside of the apparatus by controlling, by a control unit, the purge port to be on and the metering port to be off in the three-way valve when the body is at a first threshold temperature,
transporting the evaporated moisture to the Karl-Fischer unit by controlling, by the control unit, the purge port to be off and the metering port to be on when the body is at a second threshold temperature that is higher than the first threshold temperature,
transporting the evaporated moisture to the Karl-Fischer unit by controlling, by the control unit, the purge port to be off and the metering port to be on when the body is at a third threshold temperature higher than the second threshold temperature, and
transporting the evaporated moisture to outside of the apparatus by controlling, by the control unit, the purge port to be on and the metering port to be off when the body is at the third threshold temperature or higher.

10. The method of claim 9 , wherein the heating of the body comprises:
heating the body from a reference temperature up to a first threshold temperature,
heating the body from the first threshold temperature up to a second threshold temperature, and
heating the body from the second threshold temperature up to a third threshold temperature.

11. The method of claim 10 , wherein the cooling of the body comprises:
introducing at least one of gas and liquid into a cooling unit positioned outside the body to cool the body to at least one temperature selected from the group consisting of the reference temperature and the first threshold temperature.

12. The method of claim 10 , further comprising:
analyzing the imidization rate of the solid sample from the detected moisture content.

13. The method of claim 12 , wherein in the analyzing of the imidization rate, the imidization rate is analyzed by using the detected moisture content evaporated from the solid sample when the body is at at-least one temperature selected from the group consisting of a second threshold temperature and a third threshold temperature.

14. The method of claim 12 , wherein in the analyzing of the imidization rate, the imidization rate is calculated to correspond to a variable determined based on an equation given below,

DI
⁢

⁢

(
%
)

Assignees

• Lg Chemical Ltd

Inventors

• Han Su Youn
• Kim Byoung Hyoun
• Kim Dong Hyun
• Cho Hye Sung

Classifications

• G01N33/442

  Resins; Plastics · CPC title

• G01N25/4826

  concerning the heating or cooling arrangements (heating apparatus for chemical or physical laboratory apparatus in general B01L7/00) · CPC title

• G01N1/2042

  using a piston actuated by the pressure of the liquid to be sampled · CPC title

• G01N1/20

  for flowing or falling materials ({G01N1/2035} G01N1/12, G01N1/14 take precedence) · CPC title

• G01N25/58 Primary

  by measuring changes of properties of the material due to heat, cold or expansion · CPC title