Quality method complexometric titration nickel-cobalt-manganese content detection method

A complexometric titration and detection method technology, applied in the detection field, can solve problems such as large errors, and achieve the effect of eliminating specification errors and accurate detection

Inactive Publication Date: 2020-10-02
YINGDE KEHENG NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the case is carried out by volumetric EDTA complexometric titration, which has large errors.

Method used

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  • Quality method complexometric titration nickel-cobalt-manganese content detection method
  • Quality method complexometric titration nickel-cobalt-manganese content detection method
  • Quality method complexometric titration nickel-cobalt-manganese content detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Part I Reagents, Apparatus and Equipment

[0040]

[0041]

[0042]

[0043] The second part of the test process

[0044] Flow chart

[0045] Step 1: Titration of total nickel, cobalt and manganese by mass method

[0046] Operation process: The sample is digested under the heating condition of hydrochloric acid or aqua regia, and after diluting with pure water to a certain volume; titrate with EDTA standard solution, and calculate the total content of nickel, cobalt and manganese based on the consumption of EDTA standard titration solution.

[0047] Digestion: Weigh about 0.5g of the sample, record the sample mass m, put the sample in a 100mL beaker, add appropriate amount of hydrochloric acid or aqua regia, heat and digest in a fume hood, cover the mouth of the 100mL beaker with a watch glass, until the sample is completely digested , add an appropriate amount of pure water to dilute, and rinse the watch glass for 3-5 times;

[0048] Mass constant volume: c...

Embodiment 2

[0061] 1: titration of the total amount of nickel, cobalt and manganese by mass method, adopt the method of step 1 of embodiment 1, obtain the following results.

[0062]

[0063] 2: ICP nickel cobalt manganese component detection

[0064] Standard Curve Development

[0065] 2.1 Nickel standard solution spectral characteristic peaks and curves, such as figure 1 and figure 2 ;

[0066] 2.2 Spectral characteristic peaks and curves of cobalt standard solution, such as image 3 and Figure 4 ;

[0067] 2.3 Spectral characteristic peaks and curves of manganese standard solution, such as Figure 5 and Figure 6 ;

[0068] The test results of the original ICP component of the sample are as follows:

[0069]

[0070] Accurate component results after calculation

[0071]

Embodiment 3

[0073] This embodiment mainly investigates the influence of the selection of the buffer solution on the measurement accuracy of the mass method.

[0074] The nickel-cobalt-manganese standard solution adopted in the present embodiment is: a standard solution with a total concentration of nickel, cobalt and manganese of 60%;

[0075] 3.1 The influence of ammonia-ammonium chloride buffer solution on the total amount of nickel, cobalt and manganese.

[0076] The experimental method of this step is the same as step 1 of Example 1, and the pH value is adjusted to 9.5-10.5;

[0077] The results obtained by parallel testing 3 times by this method are: the total concentration of nickel, cobalt and manganese is 60.11%, 60.12%, 60.15%, and the average value is 60.13%;

[0078] 3.2 The influence of borax buffer solution on the total amount of nickel, cobalt and manganese.

[0079] The experimental method of this step is the same as step 1 of Example 1, and the pH value is adjusted to 9....

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Abstract

The invention belongs to the field of detection, and particularly relates to a mass method complexometric titration nickel-cobalt-manganese content detection method. The method comprises the followingsteps: 1, digesting and diluting a battery material containing nickel, cobalt and manganese to a set mass constant volume, performing titrating by using an EDTA standard solution, and calculating thetotal content of nickel, cobalt and manganese according to the amount of the consumed EDTA standard titration solution; 2, dissolving the battery material containing nickel, cobalt and manganese by adopting acid, and detecting the proportion of nickel, cobalt and manganese through an inductively coupled plasma emission spectrum ICP; 3, calculating the contents of nickel, cobalt and manganese according to the result of the step 1 and the result of the step 2. The method has the advantages that multiple tiny influence factors such as actual operation constant volume, pipetting volume and measuring tool specification errors, environment temperature and volume relation factors, measuring tool solution wall sticking residues and influences, tiny variation factors of volume caused by degradation and co-dissolution of digestion acid concentration and the like are eliminated; meanwhile, the accurate total amount and weight of the nickel-cobalt-manganese hydroxide are accurately detected.

Description

technical field [0001] The invention relates to the field of detection, in particular to a method for detecting the content of nickel, cobalt and manganese by mass method complexometric titration. Background technique [0002] The main reason for the instability of ingredients in the production of cathode materials in the lithium battery industry is that the main content of nickel, cobalt, and manganese in the precursor fluctuates greatly. The error range of the same batch of different constant volume liquids is 0.4-0.6%, which seriously affects the batching process in the production of cathode materials. Calculation of the lithium / metal (nickel-cobalt-manganese) ratio; it is easy to lead to insufficient or excessive lithium sources during the sintering process of the product; material capacity and residual lithium fluctuations. [0003] The applicant Tianjin Lishen Battery Co., Ltd. filed an invention patent application CN201510153083.2 in 2015, which disclosed a method for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/78G01N21/73
CPCG01N31/16G01N21/73G01N21/78
Inventor 李邑柯司兰杰苏柏涛万国江马真范江吴建华
Owner YINGDE KEHENG NEW ENERGY TECH CO LTD
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