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Method for measuring content of ferrous ions in Fe (II)-EDTA complexing denitration liquid

A technology for ion content and ferrous iron, which is applied in the field of analysis and detection, can solve the problems of narrow application range, inability to effectively measure the concentration of iron ions in different valence states, and high cost, and achieve the effect of ensuring accuracy.

Active Publication Date: 2020-10-09
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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Problems solved by technology

[0005] Generally, chemical analysis methods such as complexometric titration and redox titration, or instrumental analysis methods such as ICP-AES and ICP-MS cannot effectively determine the concentration components of iron ions in different valence states, and can only measure the total amount of iron ions
Moreover, although liquid chromatography coupled with inductively coupled plasma-mass spectrometry has been used in the field of environmental detection in recent years for the separation and determination of metal ions with different valence states (Cr 3+ with Cr 6+ , As 3+ with As 5+ , Fe 2+ with Fe 3+ etc.), but the current method is only suitable for the determination of metal ions that exist in the form of simple free ions in the aqueous phase
Because in the organic complex system of the denitrification solution with EDTA as the main component, both ferrous ions and ferric ions are completely complexed with EDTA to form a very stable organometallic complex, and the reaction of iron ions with EDTA The formed macromolecular complex ions completely changed the adsorption and analysis forms of iron ions in the liquid chromatographic column, which mostly exist in the simple water phase in the simple water phase in the inorganic system. The molecular structure of EDTA plays a key role in determining the flow rate of its chromatographic separation. Therefore, liquid chromatography cannot directly obtain the EDTA complex of ferrous ions and the EDTA complex of ferric ions. Effectively separate ferrous ions and ferric ions, that is, what flows out from the LC chromatographic column at the same time is still a mixture of EDTA complexes of ferrous ions and EDTA complexes of ferric ions. Therefore, The existing chromatographic detection technology can only measure the total concentration of polymorphic iron ions in the denitrification solution, and cannot effectively separate and separately measure Fe in the complex coexistence system of polymorphic iron ions and EDTA in the denitrification solution. 2+ and Fe 3+ Content
[0006] Moreover, if it is specially developed for the separation of Fe in the EDTA system 2+ with Fe 3+ The special effect chromatographic column not only has a narrow application range but also is difficult and expensive

Method used

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  • Method for measuring content of ferrous ions in Fe (II)-EDTA complexing denitration liquid
  • Method for measuring content of ferrous ions in Fe (II)-EDTA complexing denitration liquid
  • Method for measuring content of ferrous ions in Fe (II)-EDTA complexing denitration liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0052] A. Pretreatment of EDTA complex denitrification solution:

[0053] Separately take 5.0mL of EDTA complex denitrification solution (Sample No. 1) into a 100mL volumetric flask, add 15mL of water and mix well, add 10mL of 1.5g / L nickel standard solution, dilute to volume with water, cover the stopper, and place in ultrasonic vibration Shake the reaction for 30 minutes under the conditions of normal temperature and frequency of 52KHz in the container to obtain the test solution.

[0054] B. Determination of Fe by LC and ICP-AES 2+ Concentration components:

[0055] Connect the outlet port of the LC chromatographic separation column to the sample solution inlet port of the ICP-AES pneumatic nebulizer, draw 30 μL of the pretreatment solution and inject it into the high-performance liquid chromatograph, and immediately run ICP-AES to scan the sample solution from the chromatographic column. The spectral signal intensity of the Fe analysis line of each component that flows o...

Embodiment 2

[0061] Separately take 10.0mL of denitrification solution (Sample No. 2), add 50mL of water and mix evenly, add 30mL of nickel standard solution, and make up to volume with water; react with ultrasonic oscillation for 50min; extract 60μL of pretreatment solution and inject into LC. In addition, according to the same method as the method of Example 1, the preparation of denitrification sample solution, LC separation and ICP-AES determination of Fe 2+ .

Embodiment 3

[0063] Separately take 8.0mL of denitrification solution (Sample No. 3), add 40mL of water and mix evenly, then add 20mL of nickel standard solution, dilute with water, and react with ultrasonic oscillation for 40min; extract 50μL of pretreatment solution and inject it into LC. In addition, according to the same method as the method of Example 1 pretreatment preparation denitration sample solution, LC separation and ICP-AES determination of Fe 2+ .

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Abstract

The invention discloses a method for determining the content of ferrous ions in Fe (II)-EDTA complexing denitration liquid, which belongs to the technical field of analysis and detection. The invention provides a novel detection method for determining the concentration of Fe <2+> in an EDTA complexing denitration liquid in a polymorphic iron ion coexistence system, which comprises the steps of pretreating a sample solution by using a metal displacer, dissociating Fe <2+>, and determining the concentration component of Fe <2+>. According to the method, pretreatment and LC and ICP-AES are combined for use, so that the concentration component of Fe <2+> in the denitration solution under a polymorphic iron ion and EDTA complexing coexistence system can be rapidly, accurately and precisely measured, and thus denitration operation is effectively guided.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and specifically relates to a method based on high-performance liquid chromatography separation technology and inductively coupled plasma atomic emission spectroscopy detection technology for the determination of divalent iron under the coexistence system of multi-form iron ions in EDTA complex denitrification liquid method of ion content. Background technique [0002] Nitrogen oxides (NOx) contained in industrial flue gas X ) is one of the main pollutants in the atmosphere. It is not only the main formation factor of acid rain, but also a dangerous carcinogen, which seriously endangers the natural ecological environment and human health. In recent years, the world has paid more and more attention to NO in industrial smoke. X emission standards. Therefore, in order to meet the needs of higher and stricter emission standards for environmental protection, all industrial enterprises...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N30/06G01N30/02
CPCG01N21/73G01N30/06G01N30/02G01N2030/067
Inventor 成勇刘力维袁金红
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD