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Method for Simultaneously Determining Concentration Components of Ferric and Ferric Ions in Fe-EDTA Complex Denitrification Solution

A technology of ion concentration and ferric iron, 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, high cost, etc., and achieve the effect of ensuring accuracy

Active Publication Date: 2022-05-24
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Usually complexometric titration, redox titration and other chemical analysis methods or instrumental analysis methods such as ICP-AES and ICP-MS cannot effectively determine the concentration 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 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 Simultaneously Determining Concentration Components of Ferric and Ferric Ions in Fe-EDTA Complex Denitrification Solution
  • Method for Simultaneously Determining Concentration Components of Ferric and Ferric Ions in Fe-EDTA Complex Denitrification Solution
  • Method for Simultaneously Determining Concentration Components of Ferric and Ferric Ions in Fe-EDTA Complex Denitrification Solution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A. EDTA complex denitration solution pretreatment:

[0053] Dispense 2.5mL of EDTA complex denitration solution (sample No. 1) into a 50mL volumetric flask, add 37mL of water and mix well, add 10mL of 1.0g / L copper standard solution, dilute to volume with water, close the stopper, and place in ultrasonic vibration The reaction was oscillated for 40min at room temperature and frequency 52KHz in the device to obtain the liquid to be tested.

[0054] B. Determination of Fe by LC and ICP-AES 3+ , Fe 2+ The concentration component of:

[0055] Connect the outlet end of the chromatographic separation column of the LC to the inlet end of the sample solution of the pneumatic nebulizer of the ICP-AES, draw 30 μL of the pretreatment solution and inject it into the high performance liquid chromatograph, and immediately run the ICP-AES to measure the flow rate from the chromatographic column by scanning. The spectral signal intensity of the Fe analysis spectral lines of each com...

Embodiment 2

[0061] Dispense 1.0 mL of denitration solution (sample No. 2) into a 50 mL volumetric flask, add 10 mL of water and mix well, add 3 mL of copper standard solution, dilute with water to volume, close the stopper, and place it in an ultrasonic oscillator at room temperature and frequency The reaction was shaken at 52 KHz for 30 min, 70 μL of pretreatment solution was extracted and injected into LC, and the eluting solution flow was 1.0 mL / min. Except for this, the denitration sample solution, LC separation, and ICP-AES measurement (C(Fe 3+ )) and (C(Fe 2+ )).

Embodiment 3

[0063] Aliquot 1.5 mL of denitration solution (sample No. 3), add 15 mL of water and mix well, add 5.0 mL of Cu standard solution, and after constant volume, ultrasonically vibrate for 35 min, extract 60 μL of pretreatment solution and inject it into LC, and the flow rate of elution solution is 1.5 mL / min. Except for this, the denitration sample solution, LC separation, and ICP-AES measurement (C(Fe 3+ )) and (C(Fe 2+ )).

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Abstract

The invention discloses a method for simultaneously measuring divalent and trivalent iron ion concentration components in Fe-EDTA complex denitration solution, belonging to the technical field of analysis and detection. The invention is to realize the determination of Fe under the coexistence system of polymorphic iron ions in EDTA complex denitration solution 2+ and Fe 3+ concentration, provides a new detection method, including: the sample solution is pretreated with a metal displacer, the Fe 2+ Free: Determination of Fe separately 2+ and Fe(III)‑EDTA concentration components. Through the combination of pretreatment and LC and ICP-AES, the method can quickly, accurately and accurately measure Fe in the denitration solution in the complex coexistence system of polymorphic iron ions and EDTA. 2+ and Fe 3+ The concentration component can effectively guide the denitrification operation.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a simultaneous determination of divalent and trivalent iron ions in Fe-EDTA complex denitration solution based on the combination of high performance liquid chromatography separation technology and inductively coupled plasma atomic emission spectrometry detection technology method of concentration components. Background technique [0002] Nitrogen oxides (NO X ) is one of the main pollutants in the atmosphere, not only the main forming factor of acid rain, but also a dangerous carcinogen, seriously endangering the natural ecological environment and human health. X compliance emission. Therefore, in order to meet the needs of higher and stricter environmental protection emission standards, all industrial enterprises are faced with strengthening the control of NO X The challenge of emission, especially the inherent low temperature and high humidity of ...

Claims

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Application Information

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Patent Type & Authority Patents(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