IP Library Granted Patent US 12,693,261
Granted Patent B2
US 12,693,261 · App. 17/951,777 · Granted Jul 28, 2026

Dynamic end-point total organic fluoride measurement

Inventors: Vishnu Vardhanan Rajasekharan (Fort Collins, CO); Matthew Ryan Salzer (Loveland, CO); Russell Young (Fort Collins, CO); Benjamin James Walter (Fort Collins, CO); Jorge Gomez (Fort Collins, CO)
Assignee: Hach Company
G01N27/4163G01N27/308
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Quick Facts
Patent No.
US 12,693,261
App. No.
17/951,777
Filed
Sep 23, 2022
Granted
Jul 28, 2026
Kind
B2
Examiner
QIAN, SHIZHI
Art Unit
1795
USPC
205/775
Abstract

An embodiment provides a method for measuring an amount of total organic fluoride content of a PFAS containing sample, including: placing a sample comprising a PFAS compound in a measurement device, wherein the measurement device comprises an oxidation cell and a non-oxidation cell, wherein the oxidation cell comprises a boron-doped diamond electrode; measuring, using the measurement device, an amount of total inorganic fluoride of the sample before an oxidation; applying an electrical potential to a portion of the sample in the oxidation cell, wherein the electrical potential oxidizes the PFAS compound; measuring, using the measurement device, an amount of total organic fluoride of the sample after the oxidation to provide a measurement signal of the total organic fluoride; and determining a first derivative of the measurement signal of the total organic fluoride. Other aspects are described and claimed.

Claims (32)

1 . A method for measuring an amount of total organic fluoride of a polyfluoroalkyl substance (PFAS) compound in a sample, comprising:

placing the sample comprising the PFAS compound in a measurement device, wherein the measurement device comprises an oxidation cell and a non-oxidation cell, wherein the oxidation cell comprises a boron-doped diamond electrode;

measuring, using the measurement device, an amount of total inorganic fluoride of the sample before an oxidation;

applying an electrical potential to a portion of the sample in the oxidation cell, wherein the electrical potential oxidizes the PFAS compound;

measuring, using the measurement device, the amount of total organic fluoride of the sample after the oxidation to provide a measurement signal of the total organic fluoride;

determining a first derivative of the measurement signal of the total organic fluoride; and

comparing the first derivative to a predetermined value, wherein if the first derivative is greater than the predetermined value then adjusting the electrical potential provided to the oxidation cell.

2 . The method of claim 1 , wherein the sample circulates between the oxidation cell and the non-oxidation cell.

3 . The method of claim 1 , wherein the electric potential provides a step wise electrochemical oxidation.

4 . The method of claim 1 , further comprising determining a second derivative of the measurement signal of the total organic fluoride.

5 . The method of claim 1 , further comprising periodically turning off the electrical potential to the oxidation cell for a temperature stabilization.

6 . The method of claim 1 , further comprising periodically turning off the electrical potential to the oxidation cell to reduce an electrical noise as measured by the measurement device.

7 . The method of claim 1 , further comprising shielding the measurement device from the electrical potential applied during the oxidation.

8 . The method of claim 1 , further comprising filtering the first derivative to reduce electrical noise.

9 . The method of claim 1 , wherein the oxidation generates fluoride from a digestion of the PFAS compound using the boron-doped diamond electrode.

10 . The method of claim 1 , wherein the first derivative approaches an asymptote representing a linear background of the measurement device.

11 . The method of claim 1 , wherein the first derivative approaching an asymptote defines a dynamic end point of the oxidation.

12 . The method of claim 1 , wherein a total fluoride content equals a summation of the total inorganic fluoride and the total organic fluoride.

13 . The method of claim 1 , wherein a duration of the oxidation is determined by the first derivative reaching a threshold value.

14 . The method of claim 1 , further comprising subtracting a linear background from the measurement of the total inorganic fluoride and from the measurement of the total organic fluoride.

15 . The method of claim 14 , wherein the linear background comprises system contribution variables, wherein the system contribution variables are selected from the group consisting of: a rate constant of oxidation at the surface of the boron-doped diamond electrode, a penetration depth and diffusional rate of hydroxyl radicals, a total volume of the oxidation cell, and an exchange rate of the sample between the oxidation cell and the non-oxidation cell.

16 . The method of claim 1 , wherein the measurement device is selected from the group consisting of: an electrochemical device and an optical device.

17 . A device for measuring an amount of total organic fluoride of a PFAS compound in a sample, comprising:

a non-oxidation cell;

an oxidation cell comprising an ion selective electrode and a boron-doped diamond electrode; and

a processor;

wherein the processor is configured to:

measure an amount of total inorganic fluoride of the sample before an oxidation;

apply an electrical potential to a portion of the sample in the oxidation cell, wherein the electrical potential oxidizes the PFAS compound;

measure the amount of total organic fluoride of the sample after the oxidation to provide a measurement signal of the total organic fluoride;

determine a first derivative of the measurement signal of the total organic fluoride; and

compare the first derivative to a predetermined value, wherein if the first derivative is greater than the predetermined value then adjusting the electrical potential provided to the oxidation cell.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 23, 2022
From: RAJASEKHARAN, VISHNU VARDHANAN; SALZER, MATTHEW RYAN; YOUNG, RUSSELL; WALTER, BENJAMIN JAMES; GOMEZ, JORGE
To: HACH COMPANY
Reel/Frame 061197/0424 →
Continuity (1)
Related Publication 20240102960A1 · Mar 28, 2024
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