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Electrochemical measuring method of ferric iron content

A determination method and electrochemical technology, applied in the direction of electrochemical variables of materials, etc., can solve the problems of quantitative analysis trouble, ecological environment hazards, affecting analysis performance, etc., and achieve the effect of reducing historical residual impurities, avoiding saturation reactions, and improving sensitivity

Active Publication Date: 2012-11-21
SHAOXING MAIBAO TECH CO LTD
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  • Abstract
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Problems solved by technology

However, due to the high toxicity of mercury and its compounds themselves and the harm to the ecological environment, their application has been greatly limited in recent years, and the reproducibility of iron on mercury electrodes is poor, which affects its analytical performance [M.D.Gelado - Cabakkero, J.J. Hemandez-Brito, J.A. Herrera-Melian, et al. Electroanalysis, 1996, 8(11): 1065-1071; C. Hua, D. Jagner, L. Renman. Talanta, 1988, 35(8): 597-600]
And the anodic stripping method sensitivity on the glassy carbon electrode is poor, and situations such as multi-peak occur, and given quantitative analysis also brings trouble [P.B.Zhu, T.Nakamura, K.Izutsu.Electroanalysis, 1990,2 (1): 75 -79; Frazier W.M. Nyasulu, Horacio A. Mottola. Journal of Electroanalytical Chemistry, 1988, 239(1-2): 175-186]

Method used

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  • Electrochemical measuring method of ferric iron content
  • Electrochemical measuring method of ferric iron content
  • Electrochemical measuring method of ferric iron content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In this example, HOKUTO DENKO HAB-151 differential chronopotential analyzer and electrochemical three-electrode test system are used. A gold electrode is used as a working electrode, platinum wire is used as a counter electrode, and Ag / AgCl is used as a reference electrode. A constant current anode is used to dissolve the differential chronopotential The content of ferric iron in the samples was tested by CCSCP method. Reduction enrichment and anodic dissolution conditions are respectively: enrichment current is -4.0μA, enrichment time is 180s, resting time is 30s; during the test, anodic stripping scanning current is +5.0μA, scanning rate is 20mV s -1 , the frequency is 20Hz.

[0024] See attached figure 1 , curve 1 in the figure is for 5.0mmol L by the above method -1 Sodium acetate+80mmol L -1 Hydroxylamine hydrochloride+15.0mmol L -1 The o-phenanthroline solution contains 0.2mol L -1 The result that test obtains after the propylene carbonate extraction of TBAP;...

Embodiment 2

[0028] In this example, HOKUTO DENKO HAB-151 differential chronopotential analyzer and electrochemical three-electrode test system are used. A gold electrode is used as a working electrode, platinum wire is used as a counter electrode, and Ag / AgCl is used as a reference electrode. A constant current anode is used to dissolve the differential chronopotential The method (CCSCP) was used to determine the content of ferric iron in the spiked seawater. Reduction enrichment and anodic dissolution conditions are respectively: enrichment current is -5.0μA, enrichment time is 180s, resting time is 30s; during the test, anodic stripping scanning current is +5.0μA, scanning rate is 20mV s -1 , the frequency is 20Hz.

[0029] Fresh actual seawater samples were first filtered through 0.45 μm microporous filter paper.

[0030] See attached figure 2 , first with 5.0mmol L -1 Sodium acetate, 1.0mol L -1 NaCl, 80mmolL -1 Hydroxylamine hydrochloride, 7.5mmol L -1 The 10mL bottom solution...

Embodiment 3

[0033] According to the test method of Example 2, the iron content of the spiked river water was measured.

[0034] Fresh actual river water samples were first filtered through 0.45 μm microporous filter paper.

[0035] See attached image 3 , first with 5.0mmol L -1 Sodium acetate, 1.0mol L -1 NaCl, 80mmolL -1 Hydroxylamine hydrochloride, 7.5mmol L -1 The 10mL bottom solution of o-phenanthroline contains 0.1mol L -1 Test after the propylene carbonate extraction of TBAP, the result is shown by curve 10; In curve 10 solution, add 10mL sampling river water after treatment, adjust and keep the equilibrium concentration of each component to be: 5.0mmol L -1 Sodium acetate, 1.0mol L -1 NaCl, 80mmolL -1 Hydroxylamine hydrochloride, 7.5mmolL -1 O-phenanthroline, then containing 0.1mol L -1 After the propylene carbonate extraction of TBAP was tested, the result was shown by curve 11; -1 The concentration gradient of Fe(III) was added standardly, and test curves 12-15 were ob...

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Abstract

The invention relates to an electrochemical measuring method of ferric iron content, and an electrochemical three-electrode testing system and a constant-current anode stripping differential timing potentiometric method are adopted to carry out the measurement. The electrochemical measuring method is characterized by comprising the following steps: reducing ferric iron by hydroxylamine hydrochloride, extracting chelate Fe-[(C12H8N2)3]2+ formed by the chelation of 1,10-orthophenanthrolene into propylene carbonate organic solvent and enriching on the surface of a working electrode, obtaining a dT / dE-E differential curve by recording a function of the change of an electric potential E on the working electrode along with the testing time T and carrying out the differential processing on the function, and calculating the ferric iron content according to the height dT / dE (sV-1) of an iron response peak that is generated when an anode stripping electric potential on the differential curve is plus 400mV to plus 500mV. The invention has simple process, convenient operation, high sensitivity and low operation cost and can carry out analysis and testing on micro or trace ferric iron in natural water quality.

Description

1. Technical field [0001] The invention relates to an analysis and determination method of inorganic ions, in particular to an electrochemical analysis method, in particular to an electrochemical determination method for ferric iron content. 2. Technical background [0002] Iron is an important natural metal element in nature, widely distributed in soil, minerals, water environment, biological system, and even in the food chain. Iron can exist in the natural environment in a variety of compound states (0, II, III) and in the form of organic and inorganic substances, among which Fe(III) is the most common. In life sciences, iron is one of the essential trace elements for animals, plants and humans, and it plays an important role in the growth, metabolism, nerve conduction, enzyme activation, and anti-cancer of cells [H.Hasegawa, T .Maki, K.Asano, et al.Analytical Sciences, 2004,20(1):89-93; D.S.Yu, S.P.Liu, Z.F.Liu, et al.Chinese Journal of Geochemistry, 1995,14(2):134- 139...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/42G01N27/38
Inventor 许云辉黄晨永长幸雄
Owner SHAOXING MAIBAO TECH CO LTD
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