Analytical method for the determination of nitrogen, carbon, hydrogen and sulfur or chlorine and apparatus therefor

• US 4,401,763 A
• Filed: 11/05/1981
• Issued: 08/30/1983
• Est. Priority Date: 11/13/1980
• Status: Expired due to Term

• Current Assignee: Sumitomo Chemical Company Limited
• Original Assignee: Sumitomo Chemical Company Limited
• Inventors: Itoh, Tadamasa
• Primary Examiner(s): Turk, Arnold
• Application Number:
  US06/318,406
• Time in Patent Office: 663 Days
• Field of Search: 23/230 PC, 23/232 C, 422/78, 422/80, 436/115, 436/123, 436/124, 436/144, 436/145, 436/155, 436/158, 436/159, 436/160
• US Class Current: 436/115
• CPC Class Codes: G01N 31/12 using combustion G01N25/20 takes precedence
• CPC Class Codes: Y10T 436/176921 As part of an elemental analysis
• CPC Class Codes: Y10T 436/188 Total or elemental sulfur
• CPC Class Codes: Y10T 436/19 Halogen containing
• CPC Class Codes: Y10T 436/22 Hydrogen, per se
• CPC Class Codes: Y10T 436/23 Carbon containing

Abstract

An analytical method for the independent or simultaneous determination of any number of elements selected from the group consisting of nitrogen, carbon, hydrogen and sulfur or chlorine in samples, which comprises passing an oxygen gas through a reaction tube packed with an oxidation catalyst or oxidizing agent having a heating zone of from 800° C. to 1100° C., introducing a sample into said tube to subject it to complete combustion, uniformalizing the gas, dividing the gas into two portions, and introducing one portion in a carrier gas into a copper-reducing tube having a heating zone of from 400° C. to 700° C., determining the resulting nitrogen gas, carbon dioxide gas and steam or acetylene gas on a gas detector, while introducing the second portion in an oxygen gas into an absorption liquor, and determining the resulting sulfate or chlorine ion and, an apparatus useful therefor.

Claims

1. A method for elementary analysis by independent or simultaneous determination of any number of elements from the group consisting of nitrogen, carbon, and hydrogen and at least one element of sulfur or chlorine in samples, comprising:

passing an oxygen gas through a combustion system in a reaction tube packed with an oxidation catalyst or oxidizing agent having a heating zone maintained at a temperature of from 800°

C. to 1100°

C.;

introducing a sample into said reaction tube with circulating oxygen in a closed system, said oxygen being present in an amount sufficient to thereby subject said sample to complete combustion and said circulating oxygen uniformalizing the resulting combustion gas by continuous circulation during combustion to achieve a homogeneous combustion gas mixture;

dividing the homogeneous combustion gas mixture into first and second combustion portions in a definite volume ratio;

introducing said first combustion portion, together with a carrier gas, into a reduction tube packed with reduced copper having a heating zone maintained at a temperature of from 400°

C. to 700°

C., and detecting and determining the resulting nitrogen gas, carbon dioxide gas and steam or acetylene gas or hydrogen gas produced by contacting steam with calcium carbide or calcium hydride;

while

introducing sulfur oxide or chlorine and/or hydrogen chloride gas contained in said second combustion mixture into an absorption liquor together with oxygen gas; and

detecting and determining at least one of the resulting sulfate or chloride ion.

2. A method for elementary analysis according to claim 1, wherein the oxidation catalyst is palladium or platinum.

3. A method for elementary analysis according to claim 1, wherein the detection of nitrogen gas, carbon dioxide gas, and acetylene gas is performed by thermal conductivity, helium ionization or photointerference techniques.

4. A method for elementary analysis according to claim 1, wherein the detection of sulfur oxides is performed by specific ion electrodes, solution electroconductivity, coulometric titration, rosaniline colorimetry or barium chloride turbidimetry techniques, and the detection of hydrogen chloride or chlorine is performed by specific ion electrodes, silver nitrate turbidimetry, mercuric thiocyanate colorimetry or silver chlorate colorimetry techniques.

5. A method for elementary analysis according to claim 1, wherein the oxidizing agent is cobalt oxide or copper oxide.

6. A method for elementary analysis according to claim 5, wherein the oxidizing agent is used and at a temperature of from 800°

C. to 950°

C.

7. An apparatus for elementary analysis by independent or simultaneous determination of any number of elements from the group consisting of nitrogen, carbon and hydrogen and at least one element of sulfur or chlorine in samples comprising:

a closed combustion system for combusting a sample to be analyzed, said closed combustion system including a gas recirculation means for continuous circulation of gases contained within the combustion system, thereby uniformalizing the resulting combustion gas to achieve a homogeneous gas mixture;

an oxygen gas line-changing means for selectively alternating an oxygen gas feed to said combustion means in a closed system or to an absorption means;

a combustion gas division means for dividing the homogeneous combustion gas mixture into first and second combustion portions in a definite volume ratio and simultaneously introducing said first combustion portion of the homogeneous combustion gas mixture into a carrier gas;

a reduced copper-packed reduction means for reducing nitrogen oxides contained in the mixture of said first combustion portion and said carrier gas to nitrogen gas and simultaneously removing oxygen gas;

a gas separation means for separating the resulting gas;

a gas detection means for detecting gas thus separated;

a combustion gas absorption means for absorbing and collecting sulfur oxide or chlorine and/or hydrogen chloride gas contained in said second combustion portion; and

an absorbed gas detection means for detecting gases thus absorbed in said gas absorption means.

8. An apparatus for elementary analysis as in claim 7, wherein a gas absorption means is provided between said reduction means and said gas separation means, said gas absorption means comprising a tube packed with at least one member selected from the group consisting of a moisture absorber, a carbon dioxide gas absorber, and a converting agent for converting steam to acetylene gas or hydrogen gas.

9. An apparatus for elementary analysis as in claim 8, wherein said absorption means is packed with at least one member selected from the group consisting of calcium carbide, calcium hydride, magnesium perchlorate, and soda asbestos.

10. An apparatus for elementary analysis as in claim 7, wherein said closed combustion system includes as a combustion means a reaction tube packed with an oxidizing agent or an oxidation catalyst.

11. An apparatus for elementary analysis as in claim 10, wherein said oxidizing agent is cobalt oxide or copper oxide, or said oxidation catalyst is palladium or platinum.

12. An apparatus for elementary analysis as in claim 7, wherein said combustion gas absorption means comprises an absorption liquor.

13. An apparatus for elementary analysis as in claim 12, wherein said absorption liquor comprises aqueous solutions containing sodium chloride and mercuric chloride, aqueous hydrogen peroxide, or water.