Systems and methods for high temperature, high pressure isothermal calorimetry

Patent metadata

Field	Value
Publication number	US-12055504-B2
Application number	US-202017037902-A
Country	US
Kind code	B2
Filing date	Sep 30, 2020
Priority date	Sep 30, 2019
Publication date	Aug 6, 2024
Grant date	Aug 6, 2024

Abstract

Methods and systems for high temperature, high pressure isothermal calorimetry are disclosed. The calorimetric system includes an ampoule having a body portion and a lid configured to completely seal the body portion. One or more solid reagents are disposed in the body portion of the ampoule, and a container is disposed within the body portion of the ampoule. The container separately stores one or more fluids for mixing with the one or more solid reagents. The lid is spring loaded and wound by a winding key for stirring the one or more solid reagents with the one or more fluids to form a homogenous mixture.

First claim

The invention claimed is:

1. A calorimetric system comprising:
an ampoule having a body portion and a lid configured to completely seal the body portion, the lid comprising,
the first sprocket wheel,
a first coil spring coupled to the first sprocket wheel, and
a first shaft coupled to the first sprocket wheel;

one or more solid reagents disposed in the body portion of the ampoule;
a pressure valve coupled to one or more external pumps and configured to increase or decrease pressure within the ampoule; and
a container disposed within the body portion of the ampoule, the container separately storing one or more fluids for mixing with the one or more solid reagents.

2. The calorimetric system according to claim 1 ,
wherein the first spring is configured to be wound by a first winding key.

3. The calorimetric system according to claim 2 , wherein the lid further comprises:
a second sprocket wheel;
a second coil spring coupled to the second sprocket wheel; and
a second shaft coupled to the second sprocket wheel, wherein the second spring is configured to be wound by a second winding key.

4. The calorimetric system according to claim 3 , wherein the lid further comprises:
one or more blades coupled to a bottom end of the second shaft, wherein the one or more blades are configured to mix the one or more solid reagents with one or more fluids as the second spring unwinds.

5. The calorimetric system according to claim 3 , wherein the second sprocket wheel is locked from rotating using a ratchet coupled to the first sprocket wheel, and wherein the ratchet is released by a pin associated with the first sprocket wheel.

6. The calorimetric system according to claim 1 , wherein the body portion has a substantially cylindrical shape and the lid has a corresponding shape for completely sealing the body portion.

7. The calorimetric system according to claim 1 , wherein the body portion comprises glass or stainless steel.

8. The calorimetric system according to claim 1 , wherein the lid comprises glass or stainless steel.

9. The calorimetric system according to claim 1 , wherein the container comprises glass or stainless steel.

10. A method for performing isothermal calorimetry, the method comprising:
providing a predetermined amount of a solid reagent in an ampoule, the ampoule having a body portion and a lid configured to completely seal the body portion;
providing a predetermined volume of a fluid and a reagent within a container, the container positioned within the body portion of the ampoule;
closing the lid over the body portion of the ampoule;
placing the ampoule within a calorimeter;
winding a sprocket wheel coupled to the lid, the sprocket wheel coupled to a shaft comprising one or more blades at a bottom end of the shaft, the one or more blades configured to mix the solid reagent with the fluid; and
measuring a heat flow within the ampoule.

11. The method according to claim 10 , wherein
the reagent is solid reagent, the method further comprising forming a homogeneous mixture with the reagent and the liquid.

12. The method according to claim 10 , further comprising:
analyzing one or more characteristics of the solid reagent based on the measured change.

13. The method according to claim 10 , further comprising:
changing pressure within the ampoule via a pressure valve coupled to the lid of the ampoule, wherein the pressure valve is coupled to one or more external pumps.

14. A method for performing isothermal calorimetry comprising:
obtaining an ampoule having a body portion, a container in the body portion, a lid configured to completely seal the body portion;
disposing a reagent in the body portion;
disposing a fluid in the container;
placing the ampoule within a calorimeter;
mixing the reagent with the fluid;
measuring a heat flow within the ampoule; and
delaying the step of mixing the reagent with the fluid for a period of time after the step of placing the ampoule within the calorimeter.

15. The method of claim 14 , wherein the step of delaying comprises using a mechanical timer comprising a first spring and wherein the step of mixing comprises using a blade that is driven by a second spring.

16. The method of claim 14 , further comprising pressurizing the ampoule through a pressure valve provided in the lid.

Assignees

• Saudi Arabian Oil Co

Inventors

• Musso Simone

Classifications

• G01N25/26

  using combustion with oxygen under pressure, e.g. in bomb calorimeter · CPC title

• G01K17/00

  Measuring quantity of heat (measuring temperature by calorimetry G01K3/00 - G01K11/00; specially adapted for measuring thermal properties of materials, e.g. specific heat, heat of combustion G01N) · CPC title

• B01L2300/168

  Specific optical properties, e.g. reflective coatings · CPC title

• G01N25/486 Primary

  Sample holders · CPC title

• G01N33/383 Primary

  Concrete or cement · CPC title