Hybrid calorimeter cell

Patent metadata

Field	Value
Publication number	US-12259282-B2
Application number	US-202117521966-A
Country	US
Kind code	B2
Filing date	Nov 9, 2021
Priority date	Aug 31, 2017
Publication date	Mar 25, 2025
Grant date	Mar 25, 2025

Abstract

A calorimeter and method is also provided, including a sample cell, a reference cell, a thermostat in thermal communication with the sample cell and the reference cell, a first conductive wire, the first conductive wire having a first end connected to the thermostat and a second end connected to the sample cell, and a second conductive wire, the second conductive wire having a first end connected to the thermostat and a second end connected to the reference cell.

First claim

What is claimed is:

1. A calorimeter comprising:
a sample cell;
a reference cell;
a thermostat in thermal communication with the sample cell and the reference cell;
a thermoelectric device (TED) sensor positioned between the sample cell and the reference cell;
a first conductive wire having a first end connected to the thermostat and a second end connected to the sample cell; and
a second conductive wire having a first end connected to the thermostat and a second end connected to the reference cell.

2. The calorimeter of claim 1 , wherein the first end of the first conductive wire and the first end of the second conductive wire are each connected to the thermostat at a same location on the thermostat.

3. The calorimeter of claim 1 , wherein the first end of the first conductive wire and the first end of the second conductive wire are each connected to the thermostat at different locations on the thermostat.

4. The calorimeter of claim 1 , further comprising:
a cooling TED connected to the sample cell; and
a passive thermal shield enclosing the sample cell, the reference cell, the TED sensor, and the cooling TED.

5. The calorimeter of claim 1 , wherein the first and second conductive wires are each insulated by an insulating material to prevent heat loss from the first and second conductive wires.

6. The calorimeter of claim 1 , wherein the reference cell has a chemically inert cell body and a thermally conductive layer attached to the chemically inert cell body of the reference cell.

7. The calorimeter of claim 6 , wherein the second end of the second conductive wire is attached to the thermally conductive layer of the reference cell.

8. The calorimeter of claim 1 , wherein the sample cell has a chemically inert cell body and a thermally conductive layer attached to the chemically inert cell body.

9. The calorimeter of claim 8 , wherein the chemically inert cell body has a wall thickness less than 0.0625 inches.

10. The calorimeter of claim 8 , wherein the second end of the first conductive wire is attached to the thermally conductive layer attached to the cell body of the sample cell.

11. A method comprising:
providing the calorimeter of claim 1 ; and
establishing a highly thermally conductive path from the thermostat to the sample cell and reference cell with the first and second conductive wires.

12. The method of claim 11 , further comprising:
adjusting a power to a sample heater of the sample cell to drive a temperature difference measured by a thermoelectric sensor positioned between the sample cell and the reference cell to zero.

13. The method of claim 12 , further comprising:
measuring a differential heat flow to a sample in the sample cell with respect to the reference cell by determining an additional power needed to drive the temperature difference measured by the thermoelectric sensor positioned between the sample cell and the reference cell to zero.

14. A method of configuring a calorimeter comprising:
providing the calorimeter, the calorimeter including:
a sample cell,
a reference cell,
a thermostat in thermal communication with the sample cell and the reference cell,
a thermoelectric (TED) sensor positioned between the sample cell and the reference cell,
a first conductive wire having a first end connected to the thermostat and a second end connected to the sample cell, and
a second conductive wire having a first end connected to the thermostat and a second end connected to the reference cell;

attaching a thermally conductive layer to an exterior surface of a cell body of the sample cell, the cell body comprising a chemically inert material; and
connecting the thermally conductive layer to the thermostat of the calorimeter with the first conductive wire.

15. The method of claim 14 , wherein the chemically inert material is nickel-molybdenum alloy or a nickel-chromium-molybdenum alloy.

16. The method of claim 14 , wherein the thermally conductive layer is comprised of a material selected from the group consisting of: gold, aluminum, copper, and silver.

17. The method of claim 14 , wherein the cell body has a wall thickness less than 0.0625 inches, formed from the chemically inert material.

18. The method of claim 14 , wherein the reference cell includes a thermally conductive layer and a cell body including a chemically inert material, the method further comprising:
connecting the thermally conductive layer of the reference cell to the thermostat of the calorimeter with the second conductive wire.

Assignees

• Waters Technologies Corp

Inventors

• Russell Donald J
• Arnerich Anthony E
• Serrell David

Classifications

• G01N25/4866

  by using a differential method · CPC title

• G01N25/486

  Sample holders · CPC title

• G01N25/4853

  Details · CPC title

• G01K17/04 Primary

  Calorimeters using compensation methods {, i.e. where the absorbed or released quantity of heat to be measured is compensated by a measured quantity of heating or cooling} · CPC title