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Method for detecting content of residual EDTA in lithium fluoride

A detection method and technology of lithium fluoride, applied in the field of chemical quantitative detection and analysis, can solve the problems of no quantitative detection of EDTA, inability to detect the residual amount of EDTA, etc., and achieve a low detection limit, small relative deviation and high stability. Effect

Active Publication Date: 2019-01-15
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for lithium fluoride products with high metal ion content and many types (lithium fluoride contains sodium, potassium, magnesium, calcium, copper, ammonium ions, etc.), high performance liquid chromatography cannot detect fluoride. All EDTA residues in lithium products, there are currently no relevant literature reports on how to quantitatively detect EDTA residues in lithium fluoride products

Method used

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  • Method for detecting content of residual EDTA in lithium fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Prepare COD quick tester and intelligent digester; prepare reagent D and reagent E; set digestion parameters: run at 160°C for 10 minutes.

[0038] (2) Prepare 10, 50, 100, 200, 1000 mg / L EDTA standard solutions, shake well and set aside.

[0039] (3) Take 2.5mL of EDTA standard solutions of different concentrations in each test tube in turn, add D reagent and E reagent to each test tube successively, shake well, put the test tube carefully into the digestion apparatus for digestion for 10 minutes, after the digestion is completed , Take out the test tube carefully and put it in the test tube rack to cool in air for 2 minutes.

[0040] (4) After the cooling is completed, add 2.5 mL of ultrapure water to each test tube and shake well.

[0041] (5) Pour the solution in the test tube into a 3cm cuvette, put it into the speed measuring instrument and read the COD value by colorimetry at the COD gear, record the experimental data, and obtain the COD value corresponding ...

Embodiment 2

[0044] (1) Prepare COD quick tester and intelligent digester; prepare reagent D and reagent E; set digestion parameters: run at 160°C for 10 minutes.

[0045] (2) Prepare 10, 50, 100, 200, 1000 mg / L EDTA standard solutions, shake well and set aside.

[0046] (3) Take 2.5mL of EDTA standard solutions of different concentrations in each test tube in turn, add D reagent and E reagent to each test tube successively, shake well, put the test tube carefully into the digestion apparatus for digestion for 10 minutes, after the digestion is completed , Take out the test tube carefully and put it in the test tube rack to cool in air for 2 minutes.

[0047] (4) After the cooling is completed, add 2.5 mL of ultrapure water to each test tube and shake well.

[0048] (5) Pour the solution in the test tube into a 3cm cuvette, put it into the speed measuring instrument and read the COD value by colorimetry at the COD gear, record the experimental data, and obtain the COD value corresponding ...

Embodiment 3

[0051] (1) Prepare COD quick tester and intelligent digester; prepare reagent D and reagent E; set digestion parameters: run at 165°C for 10 minutes.

[0052] (2) Prepare 10, 50, 100, 200, 1000 mg / L EDTA standard solutions, shake well and set aside.

[0053] (3) Take 2.5mL of EDTA standard solutions of different concentrations in each test tube in turn, add D reagent and E reagent to each test tube successively, shake well, put the test tube carefully into the digestion apparatus for digestion for 10 minutes, after the digestion is completed , Take out the test tube carefully and put it in the test tube rack to cool in air for 2 minutes.

[0054] (4) After the cooling is completed, add 2.5 mL of ultrapure water to each test tube and shake well.

[0055] (5) Pour the solution in the test tube into a 3cm cuvette, put it into the speed measuring instrument and read the COD value by colorimetry at the COD gear, record the experimental data, and obtain the COD value corresponding ...

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Abstract

The invention relates to a method for detecting the content of residual EDTA in lithium fluoride. The method comprises the following steps that S1, a plurality of sets of EDTA standard solutions withdifferent gradient concentrations are prepared; S2, the EDTA standard solutions with the different gradient concentrations are taken in an equal volume mode to be added into containers correspondingly, a concentration-known regent D and a concentration-known agent E which have the same volume are added into all the containers, dissolving is conducted at 150-170 DEG C, and then cooling is conducted; S3, solutions are transferred to cuvettes and placed into a COD tachymeter, color comparison is conducted, and COD values are read and recorded; S4, according to recorded data, fitting is conductedto obtain an EDTA concentration-COD value standard curve; S5, to-be-detected sample solutions are prepared from lithium fluoride samples, the to-be-detected sample solutions replace the standard solutions in the steps S2-S3 to conduct operation in the steps S2-S3, and COD values corresponding to the to-be-detected sample solutions are recorded; and S6, the COD values obtained in the step S5 are substituted into the standard curve in the step S4, the concentrations of the EDTA in the to-be-detected sample solutions are obtained, and the residual quantity of the EDTA in the lithium fluoride samples are calculated according to the concentrations. The method has the advantages of good determination repeatability, small relative deviation and low detection limit.

Description

technical field [0001] The invention relates to the technical field of chemical quantitative detection and analysis, in particular to a detection method for residual EDTA content in lithium fluoride. Background technique [0002] Lithium fluoride, as an important lithium-based basic material, has been widely used in many aspects, especially as a synthetic raw material for lithium hexafluorophosphate (LiPF6), which is currently the most widely used. Lithium fluoride with low metal ion content can be prepared by industrial grade lithium carbonate through a series of processes. In order to further reduce the content of metal ions in lithium fluoride, mainly calcium ion content, a small amount of sodium EDTA will be added in the production process Salt to reduce the content of calcium metal ions in the product, but the residual EDTA in the final product also needs to be controlled. The residual EDTA will directly affect the quality of the product in the next step of the combined...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N1/44
CPCG01N1/44G01N21/78
Inventor 赵经伟程泽英殷松南信勇
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD