Method of determining chemical oxygen demand (COD) for high chloride samples

Patent metadata

Field	Value
Publication number	US-12235255-B2
Application number	US-201917253503-A
Country	US
Kind code	B2
Filing date	Jun 19, 2019
Priority date	Jul 4, 2018
Publication date	Feb 25, 2025
Grant date	Feb 25, 2025

Abstract

The present invention provides a method of determining chemical oxygen demand (COD) for a sample with a high concentration of chloride. The method includes obtaining the sample, determining a concentration of chloride in the sample to obtain a known concentration of chloride in the sample, dosing an amount of the sample, an acid and an oxidizing agent into a container to obtain an analyte, heating the container containing the analyte, photometrically determining a preliminary chemical oxygen demand (COD) of the analyte in an analytic device, and correcting for the high concentration of chloride using a chloride correction to obtain the chemical oxygen demand (COD).

First claim

The invention claimed is:

1. A method of determining chemical oxygen demand (COD) for a sample comprising a high concentration of chloride, the method comprising:
obtaining the sample;
determining a concentration of chloride in the sample to obtain a known concentration of chloride in the sample, wherein the known concentration of chloride is in a range from about 5,000 mg/L to about 20,000 mg/L;
dosing an amount of the sample, an acid and an oxidizing agent into a cuvette to obtain an analyte, wherein the dosing comprises pre-dosed reagents of the acid and the oxidizing agent in the cuvette;
heating the cuvette containing the analyte;
photometrically determining a preliminary chemical oxygen demand (COD) of the analyte in the cuvette in an analytic device; and
correcting the preliminary chemical oxygen demand (COD) using a chloride correction, to obtain the chemical oxygen demand (COD) and based upon a previously determined calibration value of the cuvette.

2. The method as recited in claim 1 , further comprising:
cooling, prior to the photometrically determining, the cuvette containing the analyte.

3. The method as recited in claim 1 , wherein, the acid is sulfuric acid (H2SO4);
the oxidizing agent is potassium dichromate (K 2 Cr 2 O 7 );
the heating of the cuvette is to a temperature of from about 120 to about 180° C. for 15 to 150 min.; and
the analytic device is a photometer.

4. The method as recited in claim 1 , wherein the cuvette further comprises mercury (II) sulfate (HgSO 4 ).

5. The method as recited in claim 4 , wherein: the dosing of at least one of the acid, the oxidizing agent and the mercury (II) sulfate into the cuvette occurs prior to the dosing of the amount of the sample into the cuvette.

6. The method as recited in claim 1 , further comprising:
at least one of manually inputting and manually confirming the chloride correction by a user.

7. The method as recited in claim 1 , wherein the chloride correction is based on at least one of a table, a graph, or a mathematical formula.

8. A method of determining chemical oxygen demand (COD) for a sample comprising a high concentration of chloride, the method comprising:
obtaining the sample;
determining a concentration of chloride in the sample to obtain a known concentration of chloride in the sample, wherein the known concentration of chloride is ≥20,000 mg/L;
diluting the sample prior to a dosing step;
dosing an amount of the sample, an acid and an oxidizing agent into a cuvette to obtain an analyte, wherein the dosing comprises pre-dosed reagents of the acid and the oxidizing agent in the cuvette;
heating the cuvette containing the analyte;
photometrically determining a preliminary chemical oxygen demand (COD) of the analyte in the cuvette in an analytic device; and
correcting the preliminary chemical oxygen demand (COD) using a chloride correction, to obtain the chemical oxygen demand (COD) and based upon a previously determined calibration value of the cuvette.

Assignees

• Hach Lange Gmbh

Inventors

• Hünig Isabel
• Schulz Carsten
• Guthmann Helga
• Kloos Ralf

Classifications

• G01N21/31 Primary

  Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry {(G01N21/72 takes precedence)} · CPC title

• G01N2201/121

  Correction signals · CPC title

• G01N33/1806 Primary

  Biological oxygen demand [BOD] or chemical oxygen demand [COD] · CPC title