ADAPTIVE RANGE TITRATION SYSTEMS AND METHODS

• US 20190317063A1
• Filed: 04/16/2019
• Published: 10/17/2019
• Est. Priority Date: 04/16/2018
• Status: Active Grant

• Current Assignee: Ecolab USA Incorporated (Ecolab, Inc.)
• Original Assignee: Ecolab USA Incorporated (Ecolab, Inc.)
• Inventors: Kraus, Paul R., Ryther, Robert J.
• Granted Patent: US 11,397,170 B2
• Time in Patent Office: Days
• CPC Class Codes: G01N 31/16 using titration
• CPC Class Codes: G01N 35/00722 Communications; Identification
• CPC Class Codes: G01N 35/1002 Reagent dispensers

Abstract

Systems for quantifying a target analyte concentration in a process solution are provided and can be used, for example, in methods for quantifying a target analyte concentration. These systems and methods include continuous automated titration methods that use titration chemistries to measure the target analyte concentration in the process solution. The method steps provide for efficient and robust automated titration methods for a variety of target analytes and can include methods that provide for methods that provide a dynamic range for measurement of target analyte concentrations.

Claims

1. A method for controlling a chemical process comprising

controlling a process controller communicatively coupled to a chemical reagent pump injecting a chemical reagent into the chemical process through a chemical reagent injection pump;

controlling a sample controller communicatively coupled to a sample pump, a titrant pump, and a detector,

the controller initiating a series of titration processes repeated one after the other with a set time interval between titration processes,

each titration process comprising;

collecting a sample from the chemical process;

controlling the sample pump to set the flow rate of the sample as a continuously flowing and refreshed sample stream in a reaction manifold,

controlling the titrant pump for pumping the titrant into the reaction manifold to contact the continuously flowing and refreshed sample stream and successively altering a titrant concentration in the reaction manifold and receiving a response from the detector for each different titrant concentration, and

identifying a titration endpoint for the reaction between the analyte and the titrant and determining an analyte concentration in the sample stream;

analyzing sample variation by determining the difference between a current analyte concentration and a previous analyte concentration from a previous titration process, and comparing the difference between the current analyte concentration and the previous analyte concentration from the previous titration to a specified minimum analyte concentration variation range,

when the difference between the analyte concentration and the analyte concentration from the previous titration is greater than the specified minimum analyte concentration variation range, the controller reduces the set time interval between titration processes.

2. The method of claim 1, further comprising storing the specified minimum analyte concentration variation range and the analyte concentration from two or more of the series of titration processes in a memory device.

3. The method of claim 2, further comprising controlling the process controller communicatively coupled to the memory device and the chemical reagent injection pump.

4. The method of claim 3, wherein when the difference between the analyte concentration and the analyte concentration from the previous titration is greater than the specified minimum analyte concentration variation range, then the process controller increases or decreases an injection rate of the chemical reagent injection pump.

5. The method of claim 4, wherein when the difference between the analyte concentration and the analyte concentration from the previous titration is greater than the specified minimum analyte concentration variation range and the analyte concentration is greater than the analyte concentration from the previous titration, the injection rate of the chemical reagent injection pump is decreased.

6. The method of claim 4, wherein when the difference between the analyte concentration and the analyte concentration from the previous titration is greater than the specified minimum analyte concentration variation range and the analyte concentration is less than the analyte concentration from the previous titration, the injection rate of the chemical reagent injection pump is increased.

7. The method of claim 3, wherein when the difference between the analyte concentration and the analyte concentration from the previous titration is not greater than the specified minimum analyte concentration variation range, then the process controller does not change an injection rate of the chemical reagent injection pump.

8. The method of claim 1, wherein the titrant concentration is altered by changing the flow rate of the titrant.

9. The method of claim 1, wherein the set time interval between titration processes is from about 10 seconds to about 2 hours.

10. The method of claim 1, wherein the set time interval between titration processes is from about 5 minutes to about 1 hour.

11. The method of claim 8, wherein the set time interval between titration processes is reduced by a factor of from about 1.5 to about 10.

12. The method of claim 8, wherein the set time interval between titration processes is reduced by a factor of from about 1.5 to about 4.

13. The method of claim 1, wherein the specified minimum analyte concentration variation range is ±

2.5% to about ±

25% based on the measured analyte concentration.

14. The method of claim 1, wherein the specified minimum analyte concentration variation range is from about 1 ppm to about 4000 ppm.

15. The method of claim 1, further comprising when the difference between the analyte concentration and the analyte concentration from the previous titration is less than or equal to the specified minimum analyte concentration variation range, the controller increases the set time interval between titration processes.

16. The method of claim 15, wherein the set time interval between titration processes is increased by a factor from about 1.5 to about 10.

17. The method of claim 15, wherein the set time interval between titration processes is increased to an original value.

18. The method of claim 1, wherein the chemical process is a hydraulic fracturing process, a meat processing process, or a vegetable processing process.

19. The method of claim 1, wherein the chemical reagent is a biocide, an acid, a base, a hardness reagent, or a detergent.

20. A method of controlling an automated titration system comprising

controlling a controller communicatively coupled to a sample pump, a titrant pump, and a detector,

the controller initiating a series of titration processes repeated one after the other with a set time interval between titration processes,

each titration process comprising:

controlling the sample pump to set the flow rate of a continuously flowing and refreshed sample stream in a reaction manifold,

controlling the titrant pump for pumping the titrant into the reaction manifold to contact the continuously flowing and refreshed sample stream and successively altering a titrant concentration in the reaction manifold and receiving a response from the detector for each different titrant concentration, and

identifying a titration endpoint for the reaction between the analyte and the titrant and determining an analyte concentration in the sample stream;

analyzing sample variation by determining the difference between a current analyte concentration and a previous analyte concentration from a previous titration process, and comparing the difference between the current analyte concentration and the previous analyte concentration from the previous titration to a specified minimum analyte concentration variation range,

when the difference between the analyte concentration and the analyte concentration from the previous titration is greater than the specified minimum analyte concentration variation range, the controller reduces the set time interval between titration processes.