A kind of assay method of trace silicon in tricobalt tetroxide

A technology of cobalt tetroxide and determination method, which is applied in material excitation analysis, thermal excitation analysis, etc., can solve the problems of high analysis results of low content silicon, complicated spectrophotometric operation process, harsh dissolution conditions, etc., and achieve stable and reliable analysis results. , Speed ​​up sample dissolution, and measure the effect of fast

Active Publication Date: 2019-08-06
LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a simple, fast and easy-to-operate analysis method for trace silicon in tricobalt tetroxide, which solves the defects of low test efficiency due to harsh dissolution conditions and long dissolution time in the original method, and spectroscopic colorimetry The operation process is complicated, and the analysis results of low silicon content are easy to be high

Method used

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  • A kind of assay method of trace silicon in tricobalt tetroxide
  • A kind of assay method of trace silicon in tricobalt tetroxide
  • A kind of assay method of trace silicon in tricobalt tetroxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Determination of silicon in standard samples of cobalt tetroxide series: standard sample 1-1 (Si%, 0.00040)

[0066] 1. Instruments and equipment used in the test:

[0067] Inductively coupled plasma optical emission spectrometer Optima 7000DV from American PE company

[0068] Microwave digestion instrument Multiwave PRO from Anton Paar, Austria

[0069] Ultrapure water machine Merck Millipore Milli-Q Reference 15

[0070] Electronic analytical balance Swiss Mettler-Toledo company XS205DU (weighing range 0.1mg ~ 220g)

[0071] 2. Reagents used in the experiment

[0072] Ultra-pure water

[0073] 36%-38% concentrated hydrochloric acid (excellent grade)

[0074] 40% hydrofluoric acid (analytical pure)

[0075] Boric acid (excellent grade)

[0076] Diyttrium trioxide (Y2O3): purity ≥99.999%

[0077] Silica, high purity 5N

[0078] Silicon standard storage solution: burn the standard silicon dioxide (not less than 99.99wt%) at 1000°C for 30min, cool and dry. Weigh...

Embodiment 2

[0106] Determination of silicon in standard samples of cobalt tetroxide series: standard sample 2-1 (Si%, 0.0010)

[0107] Weigh 2.7348g of cobalt tetroxide standard sample 2-1 and place it in a polytetrafluoroethylene digestion tank, then add 5-15mL36% hydrochloric acid and 0.1-0.5mL40% hydrofluoric acid in sequence, assemble the digestion tank, and prepare a blank sample at the same time, Place the microwave digestion jar in the microwave digestion instrument.

[0108] Turn on the microwave digestion instrument, set the program as follows: power 1400W, heating program for 5-20 minutes, after heating to 170-200°C, keep the temperature for 10-20 minutes, pressure 10-50bar, and cool for 10-20 minutes.

[0109] After the digestion program is finished, turn on the microwave digestion instrument and take out the digestion tank when the temperature display reaches below 70°C.

[0110] Add 5-15mL saturated boric acid solution, react at about 30-50°C for 10-30min to complex excess f...

Embodiment 3

[0122] Determination of silicon in standard samples of cobalt tetroxide series: standard sample 3-1 (Si%, 0.0018)

[0123] Weigh 2.7348g of cobalt tetroxide standard sample 3-1 and place it in a polytetrafluoroethylene digestion tank, then add 5-15mL of 36% hydrochloric acid and 0.1-0.5mL of 40% hydrofluoric acid in sequence, assemble the digestion tank, and prepare a blank sample at the same time, Place the microwave digestion jar in the microwave digestion instrument.

[0124] Turn on the microwave digestion instrument, set the program as follows: power 1400W, heating program for 5-20 minutes, after heating to 170-200°C, keep the temperature for 10-20 minutes, pressure 10-50bar, and cool for 10-20 minutes.

[0125] After the digestion program is finished, turn on the microwave digestion instrument and take out the digestion tank when the temperature display reaches below 70°C.

[0126] Add 5-15mL saturated boric acid solution, react at about 30-50°C for 10-30min to complex ...

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Abstract

The invention discloses a determining method for trace silicon in cobaltosic oxide. After a cobaltosic oxide sample is subjected to microwave digestion, an internal standard method is adopted for calibrating matrix interference, and an inductive coupling plasma emission spectrometer is used for determining the content of silicon in the determined sample. A test proves that the treatment for the sample according to the determining method provided by the invention only costs about 1 hour, the determining time is greatly shortened, the working efficiency is increased, the accuracy of determined silicon content result is high, the precision is excellent, the determination for trace silicon in cobaltosic oxide can be met and the determining method has the characteristics of low analysis cost, accuracy and practicality.

Description

technical field [0001] The invention belongs to a method for determining metal oxide components, and relates to a method for determining trace silicon in tricobalt tetroxide. Background technique [0002] Cobalt tetroxide is a kind of active material LiCoO for preparing lithium-ion battery positive electrode 2 common raw materials. In order to ensure that the prepared positive electrode active material LiCoO 2 To meet certain requirements, before the preparation, it is necessary to measure the content of non-cobalt elements on the raw material tricobalt tetroxide, which requires that the silicon content must be less than 0.01%. When testing the silicon content of cobalt tetroxide, it is necessary to dissolve cobalt tetroxide to form a solution. The existing method adopts polytetrafluoroethylene beaker electric heating plate hydrochloric acid, hydrofluoric acid to dissolve samples, because tricobalt tetroxide can only be slowly dissolved in hot hydrochloric acid, it genera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 曹笃盟徐艳燕邱平朱国忠韩峰庞燕
Owner LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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