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Method for determining iron content in ferrovanadium solution by EDTA complexing-hydrogen peroxide chromogenic matrix matching spectrophotometry

A hydrogen peroxide, matrix matching technology, used in the measurement of color/spectral properties, material analysis by observing the effect on chemical indicators, and analysis by chemically reacting materials, etc., to achieve high accuracy, improve sensitivity and Accurate, easy-to-use effects

Pending Publication Date: 2021-04-30
大连融科储能集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are highly pertinent, but also have certain limitations. They are mainly aimed at the detection of low-content iron as an impurity element.

Method used

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  • Method for determining iron content in ferrovanadium solution by EDTA complexing-hydrogen peroxide chromogenic matrix matching spectrophotometry
  • Method for determining iron content in ferrovanadium solution by EDTA complexing-hydrogen peroxide chromogenic matrix matching spectrophotometry
  • Method for determining iron content in ferrovanadium solution by EDTA complexing-hydrogen peroxide chromogenic matrix matching spectrophotometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Concentration confirmation of vanadium content in matrix solution for detection of iron content in vanadium-containing solution

[0046] 1.1 Instrument

[0047] UV-visible spectrophotometer

[0048] 1.2 Reagents

[0049] Concentrated hydrochloric acid: ρ1.179g / mL, concentrated nitric acid: ρ1.4g / mL, potassium sodium tartrate: AR, EDTA solution: AR 100g / L, sodium hydroxide solution: AR 150g / L, ammonia water: AR, hydrogen peroxide: AR 30%, ferric oxide: spectrally pure;

[0050] Ammonium metavanadate: vanadium content 43.49%.

[0051] 1.3 Working curve iron content range

[0052] 1.3.1 Series concentration iron standard solution preparation

[0053] Weigh the mass m 1 (0.1920g) (accurate to 0.0001g) of ferric oxide in a 250mL beaker, add 9mL concentrated hydrochloric acid and 3mL concentrated nitric acid (ie aqua regia), heat until completely dissolved, cool to room temperature, transfer to a 100mL volumetric flask ,Volume. Pipette the prepared iron standard solut...

Embodiment 2

[0076] Sulfuric acid-hydrochloric acid mixed acid iron vanadium electrolyte detection

[0077] 2.1 Instrument

[0078] UV-visible spectrophotometer

[0079] 2.2 Reagents

[0080] Concentrated hydrochloric acid: ρ1.179g / mL, concentrated nitric acid: ρ1.4g / mL, potassium sodium tartrate: AR, EDTA solution: AR 100g / L, sodium hydroxide solution: AR 150g / L, ammonia water: AR, hydrogen peroxide: AR 30%, ferric oxide: spectrally pure, ammonium metavanadate: vanadium content 43.49%.

[0081] 2.3 Drawing of standard curve

[0082] 2.3.1 Preparation of series concentration iron standard solution

[0083] Weigh the mass m 1 (0.1924g) (accurate to 0.0001g) of ferric oxide in a 250mL beaker, add an appropriate amount of 9mL concentrated hydrochloric acid and 3mL concentrated nitric acid, heat until completely dissolved, cool to room temperature, transfer to a 100mL volumetric flask, and constant volume.

[0084] Weigh the mass m 2 (0.3500g) of ammonium metavanadate in a 250mL beaker,...

Embodiment 3

[0114] Detection of Iron Content in VAlFe 69:19:12 Alloy Sample

[0115] 3.1 Instrument

[0116] UV-visible spectrophotometer

[0117] 3.2 Reagents and materials

[0118] Hydrochloric acid GR, nitric acid GR, potassium sodium tartrate AR, EDTA-2Na solution: 100g / L, sodium hydroxide solution: 120g / L, ammonia water AR, hydrogen peroxide AR, spectrally pure ferric oxide (baked at 105°C to constant weight);

[0119] Fe standard solution: 1000ug / mL, weigh 0.072g (accurate to 0.0001g) spectrally pure ferric oxide dried at 105°C for 1 hour in a 100mL beaker, add 6mL hydrochloric acid GR, 2mL nitric acid GR, heat to complete dissolve. After cooling, dissolve back to boiling, remove and cool, and dilute to 50mL;

[0120] Vanadium pentoxide: content ≥ 99.8%, iron content ≤ 0.01%, baked at 105°C to constant weight

[0121] Aluminum powder: content ≥ 99.7%, iron content ≤ 0.01%

[0122] 3.3 Preparation of standard curve

[0123] Weigh vanadium pentoxide (m V2O5 )0.617g (accurate ...

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Abstract

The invention provides a method for determining the iron content in a ferrovanadium solution by EDTA complexing hydrogen peroxide chromogenic matrix matching spectrophotometry. According to the method, EDTA, hydrogen peroxide and iron ions form a chromogenic group under the condition of an alkaline solution, a chromogenic signal is enhanced, the detection sensitivity is improved, interference of vanadium to iron detection is eliminated in a vanadium matrix matching mode, the detection accuracy is improved, accurate and rapid detection of the iron content in the ferrovanadium solution is achieved, and the method is suitable for industrial production; technical problems in the prior art are solved.

Description

technical field [0001] The invention relates to iron content determination technology, in particular to a method for determining iron content in ferrovanadium solution by EDTA complexation-hydrogen peroxide chromogenic matrix matching photometry. Background technique [0002] There are many methods for the determination of iron, including ultraviolet-visible spectrophotometry, redox titration, ICP and so on. Among them: the determination of iron content by potentiometric titration requires the iron to be completely reduced to divalent. This operation control condition is relatively harsh. When there are other redox reaction elements in the solution at the same time, it is more complicated to eliminate interference; the relative error of ICP determination of iron content is relatively large. High, and it is difficult to eliminate interference peaks. Due to low investment in equipment, simple operation, and under the condition of eliminating the influence of interfering eleme...

Claims

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Application Information

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IPC IPC(8): G01N21/33G01N21/78
CPCG01N21/33G01N21/78
Inventor 曾繁武王隆菲姜雪莲丁琳周振扬阎成友
Owner 大连融科储能集团股份有限公司
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