Elemental analysis system and method with a reactor having two metal zeolite nitrogen oxides reduction reaction zones

Patent metadata

Field	Value
Publication number	US-10656130-B2
Application number	US-201715582965-A
Country	US
Kind code	B2
Filing date	May 1, 2017
Priority date	May 17, 2016
Publication date	May 19, 2020
Grant date	May 19, 2020

Abstract

An elemental analysis system includes a reactor having at least one reduction reaction zone including a metal zeolite that can reduce nitrogen oxides (NO x ) to molecular nitrogen (N 2 ) by selective catalytic reduction. Correspondingly, a method of elemental analysis includes providing a reactor having at least one reduction reaction zone including a metal zeolite and reducing nitrogen oxides (NO x ) to molecular nitrogen (N 2 ) by selective catalytic reaction on the metal zeolite.

First claim

What is claimed is:

1. An elemental analysis system comprising: a first reactor including at least two reduction reaction zones, each reduction reaction zone including a metal zeolite that reduces nitrogen oxides (NO x ) to molecular nitrogen (N 2 ) by selective catalytic reaction, wherein an oxidation reaction zone is provided either (i) in the first reactor such that the oxidation reaction zone is located before the reduction reaction zones in a direction of gas flow through the first reactor, or (ii) in a second reactor in fluid communication with the first, the second reactor being located upstream of the first reactor in the direction of gas flow through the first reactor; and a mass spectrometer positioned downstream of the first reactor; wherein the at least two reduction reaction zones are separated from each other by a porous material.

2. The system of claim 1 , wherein the metal zeolite is a ZSM-5 type material.

3. The system of claim 1 , wherein the metal zeolite comprises a +2 oxidation state metal.

4. The system of claim 3 , wherein the +2 oxidation state metal is at least one of copper, platinum, nickel, and cobalt.

5. The system of claim 1 , wherein the metal content of the metal zeolite is in a range of between 2.1 wt % and 5.0 wt %.

6. The system of claim 1 , wherein the metal zeolite has a grain size in a range of between 0.3 mm and 2.9 mm.

7. The system of claim 1 , wherein the metal zeolite comprises carbon in an amount that is at least 70 ppm and less than 200 ppm.

8. The system of claim 1 , wherein the at least two reduction reaction zones are of substantially the same length or of successively increasing lengths in the direction of gas flow through the first reactor, the lengths being in total in a range of between 1% and 30% of a length of the first reactor.

9. The system of claim 8 , wherein the at least two reduction reaction zones are separated from each other by a length in a range of between 1% and 3% of a length of the first reactor.

10. The system of claim 1 , wherein the porous material comprises quartz or glass wool.

11. The system of claim 1 , wherein the first reactor further includes an oxygen gas inlet upstream of or into the oxidation reaction zone.

12. The system of claim 1 , wherein the oxidation reaction zone includes an oxygen-donor material.

13. The system of claim 12 , wherein the oxygen-donor material comprises at least one of chromium trioxide (Cr 2 O 3 ), tungsten trioxide (WO 3 ), copper oxide, and a mixture of copper oxide and platinum-coated aluminum oxide.

14. The system of claim 1 , further including a furnace to heat the first reactor, wherein each of the reduction reaction zones and the oxidation reaction zone are each configured to be heated to a temperature in the range of between 150° C. and 1,200° C.

15. The system of claim 14 , wherein each of the reduction reaction zones are configured to be heated to a lower temperature than the oxidation reaction zone.

16. The system of claim 1 , further including an oxygen capture zone, downstream of each of the reduction reaction zones, that comprises metallic copper, metallic platinum, metallic nickel, or metallic cobalt, or any combination thereof.

17. The system of claim 1 , wherein the oxidation reaction zone is located in the second reactor.

18. The system of claim 17 , further including a furnace to heat the first reactor to a temperature in the range of between 150° C. and 1,200° C., and a second furnace to heat the second reactor to a temperature in the range of between 150° C. and 1,200° C.

19. The system of claim 17 , wherein the second reactor further includes an oxygen gas inlet upstream of or into the oxidation reaction zone.

20. The system of claim 17 , wherein the oxidation reaction zone includes an oxygen-donor material.

21. The system of claim 20 , wherein the oxygen-donor material comprises at least one of chromium trioxide (Cr 2 O 3 ), tungsten trioxide (WO 3 ), copper oxide, and a mixture of copper oxide and platinum-coated aluminum oxide.

22. The system of claim 17 , wherein the first reactor is interfaced to a gas chromatography column located downstream of the first reactor in a direction of gas flow.

23. The system of claim 22 , wherein the gas chromatography column is interfaced to the mass spectrometer.

24. The system of claim 17 , further including an autosampler located upstream from the second reactor for introducing liquid or solid samples into the system.

25. The system of claim 1 , wherein the first reactor is interfaced to a gas chromatography column located downstream of the first reactor in a direction of gas flow.

26. The system of claim 25 , wherein the gas chromatography column is interfaced to the mass spectrometer.

27. The system of claim 1 , wherein the first reactor is interfaced to a gas chromatography column located upstream of the first reactor in a direction of gas flow.

28. The system of claim 1 , further including an autosampler located upstream from the first reactor for introducing liquid or solid samples into the system.

29. A method of elemental analysis of a sample, the method comprising:
a. introducing into an oxidation reaction zone a sample to be analyzed;
b. oxidizing the sample in the oxidation reaction zone to generate oxidized products including nitrogen oxides (NO x ) from nitrogen present in the sample;
c. reducing the nitrogen oxides to elemental nitrogen in a reactor including at least two reduction reaction zones, each of the reduction reaction zones including a metal zeolite that can reduce nitrogen oxides (NO x ) to molecular nitrogen (N 2 ) by selective catalytic reaction, the at least two reduction reaction zones being separated from each other by a porous material; and
d. analyzing the elemental nitrogen using mass spectrometry.

30. The method of claim 29 , wherein the analyzing comprises analyzing the molecular nitrogen (N 2 ) using isotope ratio mass spectrometry (IRMS) and determining therefrom an isotope ratio [14]N/[14]N, [15]N/[14]N, and [15]N/[15]N, and subsequently calculating a δ 15 N value for the nitrogen produced from the sample material.

31. The method of claim 30 , wherein in the IRMS analysis the mass 30 peak elutes simultaneously with mass 28 and mass 29 peaks.

32. The method of claim 29 , further including introducing oxygen upstream of or into the oxidation reaction zone.

33. The method of claim 29 , wherein the sample to be analyzed is introduced into the oxidation reaction zone using a liquid or solid autosampler.

Assignees

• Thermo Fisher Scient Bremen Gmbh

Inventors

• Guzzonato Antonella
• Brodie Christopher

Classifications

• G01N33/0036 Primary

  specially adapted to detect a particular component (physical analysis of gaseous biological material G01N33/497) · CPC title

• G01N30/62

  Detectors specially adapted therefor · CPC title

• G01N33/0013 Primary

  by a chemical reaction (a chemical reaction taking place or a gas being eliminated in one or more analysing channels G01N33/0024) · CPC title

• G01N30/06

  Preparation · CPC title

• G01N2030/8868

  elemental analysis, e.g. isotope dilution analysis · CPC title