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Method for measuring ferrous ion content in fe(ii)-edta complex denitrification solution

A technology of ion content and ferrous iron, applied in the field of analysis and detection, can solve the problems of narrow application range, inability to effectively separate and separate determination, high cost, and achieve the effect of ensuring accuracy

Active Publication Date: 2022-05-24
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Description
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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 measuring ferrous ion content in fe(ii)-edta complex denitrification solution
  • Method for measuring ferrous ion content in fe(ii)-edta complex denitrification solution
  • Method for measuring ferrous ion content in fe(ii)-edta complex denitrification solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A. EDTA complex denitration solution pretreatment:

[0053] Dispense 5.0 mL of EDTA complex denitration solution (sample No. 1) into a 100 mL volumetric flask, add 15 mL of water and mix, add 10 mL of 1.5 g / L nickel standard solution, dilute to volume with water, close the stopper, and place in ultrasonic vibration The reaction was oscillated for 30 min under the conditions of 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 2+ Concentration component:

[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 e...

Embodiment 2

[0061] Aliquot 10.0 mL of denitration solution (sample No. 2), add 50 mL of water and mix, add 30 mL of nickel standard solution, and make up to volume with water; ultrasonically vibrate for 50 min; extract 60 μL of pretreatment solution and inject into LC. In addition, according to the same method as Example 1, pretreatment to prepare denitration sample solution, LC separation and ICP-AES determination of Fe 2+ .

Embodiment 3

[0063] Aliquot 8.0 mL of denitrification solution (sample No. 3), add 40 mL of water and mix well, then add 20 mL of nickel standard solution, dilute to volume with water, and react with ultrasonic vibration for 40 min; extract 50 μL of pretreatment solution and inject into LC. In addition, according to the same method as Example 1, pretreatment to prepare 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 divalent iron ions in Fe(II)-EDTA complex denitration solution, and belongs 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 the EDTA complex denitration solution 2+ concentration, provides a new detection method, including: the sample solution is pretreated with a metal displacer, the Fe 2+ Free: Re-measure Fe 2+ concentration component. 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+ 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 method for determining divalent iron in a polymorphic iron coexistence system in an EDTA complex denitration solution based on a combination of high performance liquid chromatography separation technology and inductively coupled plasma atomic emission spectrometry detection technology method of ionic content. 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 o...

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