Determination of aqueous nitrate concentration

Patent metadata

Field	Value
Publication number	US-10317386-B2
Application number	US-201615223708-A
Country	US
Kind code	B2
Filing date	Jul 29, 2016
Priority date	Jul 29, 2016
Publication date	Jun 11, 2019
Grant date	Jun 11, 2019

Abstract

A method of measuring nitrate concentration in an aqueous sample includes mixing the aqueous sample with a water-soluble thioether chosen to reduce nitrate in the aqueous sample to nitrite in the presence of a water soluble catalyst, and a water soluble reagent system adapted to interact with nitrite to generate a color; measuring color generation, and correlating the color generation to nitrate concentration.

First claim

What is claimed is:

1. A method of measuring nitrate concentration in an aqueous sample, comprising:
a. mixing the aqueous sample with a water-soluble thioether chosen to reduce nitrate in the aqueous sample to nitrite in the presence of a water soluble catalyst, and a water soluble reagent system adapted to interact with nitrite to generate a color,
b. measuring color generation, and
c. correlating the color generation to nitrate concentration.

2. The method of claim 1 wherein the water-soluble thioether comprises a thioether-containing a five-membered, aromatic heterocyclic compound, a phenylalkyl thioether or a substituted phenylalkyl thioether.

3. The method of claim 1 wherein the water-soluble thioether has the formula:

wherein R 1 , R 2 , R 3 , R 4 , and R 5 are selected independently from H, and a hydrophilic group or electron density donating group, wherein at least one of R 1 , R 2 , R 3 , R 4 , and R 5 is a hydrophilic or an electron density donating group, and wherein R 6 is selected from the group consisting of a C 1 -C 6 alkyl group or a hydrophilic polymer.

4. The method of claim 3 wherein the hydrophilic polymer is a polyalkyleneoxide.

5. The method of claim 3 wherein at least one of R 1 , R 2 , R 3 , R 4 , and R 5 is —OR a wherein R a is selected from the group consisting of H, a C 1 -C 6 alkyl group, a C 1 -C 6 sulfonate terminated alkyl group, a phenyl group, and a polyalkylene oxide group, —NR b R c wherein R b and R c are selected independently from the group consisting of H, a C 1 -C 6 alkyl group, a C 1 -C 6 sulfonate terminated alkyl group, and a polyalkylene oxide group, a dihydroxybenzene group, a phenyl diamine group, a phenyl diether group, a carboxylate group, and a polyalkyleneoxide group; or R 1 and R 2 together form a chain of four or five members selected from the group of CH, CH 2 , NH, CC(O)OH or NR d , wherein R d is an C 1 -C 6 alkyl group or C 1 -C 6 sulfonate terminated alkyl group; or R 3 and R 4 together form a chain of four or five members selected from the group of CH, CH 2 , NH, CC(O)OH or NR d .

6. The method of claim 4 wherein the phenyl diamine has the formula C 6 H 3 (N(R 7 ) 2 )(N(R 8 ) 2 ), wherein R 7 and R 8 are independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl group, a sulfonate terminated C 1 -C 6 alkyl group, or a polylakyleneoxide group and the phenyl diether has the formula C 6 H 3 (O(R 9 ))(O(R 10 )), wherein R 9 and R 10 are independently selected from the group consisting of hydrogen, C 1 -C 6 alkyl group, a sulfonate terminated C 1 -C 6 alkyl group, or a polylakyleneoxide group.

7. The method of claim 4 wherein the polyalkyleneoxide comprises 4 to 1000 carbon atoms.

8. The method of claim 1 wherein the water soluble catalyst comprises MoO 2 Cl 2 (L) 2 wherein L is a hydrophilic phosphine group.

9. The method of claim 8 wherein L comprises a triphenylphosphineoxide group.

10. The method of claim 8 wherein L is trisulfonated-triphenylphosphineoxide.

11. The method of claim 8 wherein the water soluble catalyst further comprises a Cu 2+ co-catalyst.

12. The method of claim 1 wherein the water soluble reagent system is a Griess reagent system.

13. The method of claim 1 wherein the water soluble reagent system comprises aniline or an aniline derivative and a receptor species chosen to form a chromophore with nitrite.

14. The method of claim 13 wherein the aniline derivative is chosen to form a diazonium salt with nitrite.

15. The method of claim 14 wherein the aniline derivative is sulphanilic acid.

16. The method of claim 13 wherein the receptor species comprises an azo dye agent.

17. The method of claim 16 wherein the receptor species is chosen from the group consisting of N-alpha-naphthyl-ethylenediamine, genistic acid, and chromotropic acid.

18. The method of claim 1 wherein the color generation occurs in the visible light spectrum.

19. The method of claim 1 wherein the color generation is measured using at least one of: a spectrometer, a colorimeter, a photometric device, a color disc, and a color block.

20. The method of claim 1 wherein the range of nitrate detection is between 0 and 15 ppmw.

Assignees

• Hach Co

Inventors

• Macfarland Darren Kent
• Greenawalt Angella Nicholle

Classifications

• G01N21/251

  Colorimeters; Construction thereof · CPC title

• C07C323/20

  with singly-bound oxygen atoms bound to carbon atoms of the same non-condensed six-membered aromatic ring · CPC title

• C07D235/08

  Radicals containing only hydrogen and carbon atoms · CPC title

• G01N21/31

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

• C08G65/40

  from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group · CPC title