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Method for determining content of ferric iron in lithium iron phosphate

A ferric iron content technology, applied in fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of cumbersome operation and easily affected measurement results, and achieve the effect of high selectivity, high accuracy, and easy operation

Inactive Publication Date: 2013-07-31
CHANGZHOU UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is: in the prior art, for LiFePO 4 The determination method of ferric iron content in the medium is cumbersome to operate, and due to the existence of ferrous iron, the determination results are easily affected

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  • Method for determining content of ferric iron in lithium iron phosphate
  • Method for determining content of ferric iron in lithium iron phosphate
  • Method for determining content of ferric iron in lithium iron phosphate

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Embodiment Construction

[0030] The following examples are for illustrative purposes only and should not be construed as limitations on the practice of the present invention.

[0031] Solution preparation:

[0032] a. Preparation of acetic acid-sodium acetate standard buffer solution:

[0033] Take 6.0g of glacial acetic acid (HAc) and dissolve it in deionized water, and set the volume to 1000ml to obtain 0.1mol L -1 Acetic acid solution A;

[0034] Take 13.6g of sodium acetate (NaAc 3H 2 O) Dissolve in deionized water, dilute to 1000ml, get 0.1mol L -1 Sodium acetate solution B;

[0035] Mix 147.2ml of A and 52.8ml of B, and dilute to 1000ml with deionized water to obtain 0.02mol L -1 HAc-NaAc buffer solution at pH 4.2.

[0036] b. Preparation of ferric iron standard solution:

[0037]Weigh 0.1350g of FeCl 3 ·6H 2 O, 0.02mol L dissolved in the above 50ml -1 HAc-NaAc solution, then use 0.02mol·L -1 The HAc-NaAc solution was diluted 20 times to obtain 5.0×10 -4 mol L -1 Fe 3+ solution.

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Abstract

The invention provides a method for determining the content of ferric iron in a cell anode material LiFePO4. The method utilizes 2-pyridylaldehyde-p-phenyldihydrazone as a fluorescence reagent to detect the content of ferric iron in the LiFePO4 material. The result of the determination of the content of the ferric iron in LiFePO4 in the prior art is easily influenced because of the existence of ferrous iron. The method provided by the invention adopts the combination of ferric iron with a Schiff base compound 2-pyridylaldehyde-p-phenyldihydrazone to quench the fluorescence of 2-pyridylaldehyde-p-phenyldihydrazone, the attenuation intensity of the fluorescence of 2-pyridylaldehyde-p-phenyldihydrazone is in direct proportion to the concentration of ferric iron ions, and other irons comprising ferrous ion and the like do not cause the fluorescence quenching of 2-pyridylaldehyde-p-phenyldihydrazone, so the method based on the fluorescence intensity attenuation of 2-pyridylaldehyde-p-phenyldihydrazone can quantitatively detect the content of ferric iron in LiFePO4.

Description

technical field [0001] The present invention relates to the determination of a kind of trivalent iron content, particularly relate to LiFePO 4 Determination of ferric iron content in. Background technique [0002] Olivine LiFePO 4 It is a new type of lithium-ion battery cathode material developed in recent years. It has the advantages of low price, environmental friendliness, and good thermal stability, so it has received close attention from people. [0003] LiFePO 4 There are many preparation methods, such as solid-phase synthesis, liquid-phase synthesis, sol-gel method, emulsion drying method and redox method. Regardless of the method, ferrous iron or ferric iron is used as the iron source to prepare LiFePO 4 , but in LiFePO 4 In the system, due to the existence of a trace amount of ferric iron, LiFePO 4 The self-discharge of the positive electrode material increases, and the specific capacity decreases. At the same time, the dissolution of iron and the precipitatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 陈智栋曹小云王文昌曹剑瑜光崎尚利
Owner CHANGZHOU UNIV
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