Carbon measurements in aqueous samples using oxidation at elevated temperatures and pressures created by resistive heating

Patent metadata

Field	Value
Publication number	US-2023012945-A1
Application number	US-201917784602-A
Country	US
Kind code	A1
Filing date	Dec 11, 2019
Priority date	Dec 11, 2019
Publication date	Jan 19, 2023
Grant date	—

Abstract

Apparatus and methods for measuring the concentrations of organic and inorganic carbon, or of other materials in aqueous samples are described, having a reactor that is resistively heated by passing an electric current through the reactor.

First claim

1 . An apparatus for treating a liquid sample containing organic material, said apparatus comprising:
a reactor having reactor inlet and reactor outlet ports and a reactor interior for containing a liquid sample under above-ambient temperature and pressure conditions; high-pressure fluid reactor valve members at said reactor inlet and reactor outlet ports, said reactor valve members allowing fluid flow respectively into or out of the reactor interior when in an open-valve mode or, alternatively, capable of sealing the reactor interior when in a closed-valve mode; a reactor heating system comprising an electrical current source operably connected to the reactor, the electrical current source configured to pass an electrical current through the reactor to rapidly and cyclically heat the reactor interior and a liquid sample sealed in the reactor interior to a temperature of about 150° C. to 650° C. or higher, while the reactor interior and the reactor valve members maintain the sample under sealed conditions; and, a reactor cooling system adapted for rapidly and cyclically cooling the reactor interior and a reactor product sealed in the reactor interior following a heating cycle.

2 . The apparatus of claim 1 , wherein a sensor is configured to determine a temperature value of the reactor.

3 . The apparatus of claim 2 , wherein the sensor is configured to measure electromagnetic radiation.

4 . The apparatus of claim 2 , wherein the sensor is configured to measure infrared radiation.

5 . The apparatus of claim 2 , wherein the sensor is operably connected to the reactor heating system.

6 . The apparatus of claim 2 , wherein the sensor is operably connected to the reactor cooling system.

7 . The apparatus of claim 2 , wherein the reactor is comprised of titanium and its alloys, tantalum, Inconel 625, Hastelloy C-276, or combinations thereof.

8 . A method for treating a liquid sample containing organic material utilizing a liquid sample treatment apparatus, the method comprising the steps of:
providing a liquid sample treatment apparatus comprising the following features:
a reactor having reactor inlet and reactor outlet ports and a reactor interior for containing a liquid sample under above-ambient temperature and pressure conditions;
high-pressure fluid reactor valve members at said reactor inlet and reactor outlet ports, said reactor valve members allowing fluid flow respectively into or out of the reactor interior when in an open-valve mode or, alternatively, capable of sealing the reactor interior when in a closed-valve mode;
a reactor heating system comprising an electrical current source operably connected to the reactor, the electrical current source configured to pass an electrical current through the reactor to rapidly and cyclically heat the reactor interior and a liquid sample sealed in the reactor interior to a temperature of about 150° C. to 650° C. or higher, while the reactor interior and the reactor valve members maintain the sample under sealed conditions; and,
a reactor cooling system adapted for rapidly and cyclically cooling the reactor interior and a reactor product sealed in the reactor interior following a heating cycle;
mixing a known volume of the sample with one or more other liquids selected from oxidizer, acid and dilution water to form a sample mixture; flowing at least a portion of the sample mixture into the interior of the reactor, said reactor being adapted to be alternately and repeatedly opened and sealed at the reactor inlet and reactor outlet ports; sealing the portion of sample mixture in the interior of the reactor by closing the valve members at the reactor inlet and reactor outlet ports; passing an electrical current through the reactor for a time sufficient substantially to oxidize the organic material and form the reactor product; stopping the heating step and then rapidly cooling the interior of the reactor and the reactor product inside to substantially ambient conditions to form cooled liquid and gaseous reactor products; and, opening the reactor and removing the cooled liquid and gaseous reactor products form the reactor interior.

9 . The method of claim 8 , wherein the interior of the reactor and the sample portion inside is rapidly heated to a temperature between 150° C. to about 650° C.

10 . The method of claim 8 , wherein a sensor is provided, the sensor configured to measure a temperature value of the reactor.

11 . The method of claim 10 , wherein the sensor is configured to measure electromagnetic radiation.

12 . The method of claim 10 , wherein the sensor is configured to measure infrared radiation.

13 . The method of claim 8 , wherein a signal generated by the sensor is used to decide when to stop the heating step.

14 . The method of claim 8 , wherein the reactor is comprised of titanium and its alloys, tantalum, Inconel 625, Hastelloy C-276, or combinations thereof.

Assignees

• Bl Technologies Inc

Inventors

• Kosenka Paul P
• Vanhoudt Paulus J

Classifications

• B01L2300/1833

  using electrical currents in the sample itself · CPC title

• G01N33/004

  CO or CO2 · CPC title

• B01L2300/1894

  Cooling means; Cryo cooling · CPC title

• G01N1/44

  Sample treatment involving radiation, e.g. heat · CPC title

• G01N21/3504 Primary

  for analysing gases, e.g. multi-gas analysis · CPC title