CN103954617A - Method for detecting content of lithium carbonate - Google Patents
Method for detecting content of lithium carbonate Download PDFInfo
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- CN103954617A CN103954617A CN201410200406.4A CN201410200406A CN103954617A CN 103954617 A CN103954617 A CN 103954617A CN 201410200406 A CN201410200406 A CN 201410200406A CN 103954617 A CN103954617 A CN 103954617A
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Abstract
The invention discloses a method for detecting the content of lithium carbonate. The method comprises the following steps: with dried spectrum pure lithium carbonate and a to-be-tested sample, respectively dissolving lithium carbonate and the sample by virtue of deionized water, and completely dissolving lithium carbonate and the sample with the assistance of ultrasonic waves; adding methyl orange as an indicator into a lithium carbonate solution after the sample is completely dissolved, and carrying out titration by virtue of dilute H2SO4 until the solution becomes faint yellow; and after the titration, calculating the content of lithium carbonate according to the formula that the content of lithium carbonate is equal to [0.9998*M of the spectrum pure sample-C of H2SO4*M of Li2CO3*(V of H2SO4 spectrum pure sodium carbonate-V of H2SO4 to-be-tested sodium carbonate)]/M of the to-be-tested sample*100%. The method is used for testing the content of lithium carbonate in a sample and has the advantages that the operation is simple, the detection time is short, a titration end point is easily judged, the error is reduced, the influences of external conditions such as temperature and humidity are small, the toxicity of a utilized reagent is low, and the operation is safe.
Description
Technical field
The present invention relates to a kind of detection method of lithium compound, be specifically related to a kind of detection method of lithium carbonate content.
Background technology
Lithium carbonate is the basic material of producing lithium compound and lithium metal, is one of most important product in lithium industry.Lithium carbonate is widely used in the fields such as pottery, lithium battery, pharmacy, food, metal smelt.
Along with the application of lithium carbonate in lithium battery, the detection of high-purity carbonic acid lithium product is more and more important.The method of existing detection lithium carbonate content is " hydrochloric titration ", usings methyl red-bromcresol green as indicator, and lithium carbonate solution, through watery hydrochloric acid titration, forms lithium chloride, by measuring the consumption of watery hydrochloric acid, calculates the lithium carbonate content in testing sample.The method exists titration end-point to be difficult to judgement, and in solution, residual carbon dioxide will make titration error amplify, and titration results is subject to the external conditions such as temperature, humidity to affect the defects such as large.The method exist length consuming time, personal error large, be subject to ectocine large, be unfavorable for high precision and fast detecting.
Summary of the invention
In order to overcome the deficiency existing in existing lithium carbonate detection method of content, the detection method that the object of this invention is to provide a kind of lithium carbonate content, this method is simple to operate, cost is low, consuming time few, and detection efficiency is high, is subject to the external conditions such as temperature, humidity to affect little.
Object of the present invention is achieved through the following technical solutions:
A detection method for lithium carbonate content, is characterized in that the method comprises the following steps:
(1) take respectively the dry spectroscopic pure lithium carbonate of identical weight and treat test sample lithium carbonate sample, in 250-350 ℃ of dry 2-3h (constant weight), and in exsiccator, being cooled to room temperature;
(2) respectively with deionized water by spectroscopic pure lithium carbonate and treat that test sample lithium carbonate sample dissolves completely;
(3) until spectroscopic pure lithium carbonate with after test sample lithium carbonate sample dissolves respectively completely, respectively to spectroscopic pure lithium carbonate solution with treat to add 2-5 to drip methyl orange indicator in test sample lithium carbonate sample solution, with dilute sulfuric acid be titrated to faint yellow till;
(4), after titration completes, be calculated as follows lithium carbonate content:
Wherein, spectroscopic pure lithium carbonate content is 99.98% (demarcating), C
h2SO4for H
2sO
4amount of substance concentration, mol/L; V
h2SO4for the volume of dilute sulfuric acid that titration consumes, L; M
li2CO3for the molal weight of lithium carbonate, 73.89g/mol; M
spectroscopic pure samplefor the quality of taken spectroscopic pure sample, g; M
testing samplefor the quality of taken sample to be measured, g.
In the present invention, under ultrasound wave is auxiliary, adopt deionized water dissolving lithium carbonate sample.The concentration of dilute sulfuric acid is 0.01-0.20mol/L.Treat in test sample lithium carbonate sample that lithium carbonate content is more than 90%.
In the present invention, preferred detecting step is: get respectively 5.0000g spectroscopic pure lithium carbonate and treat test sample lithium carbonate sample, respectively at 300 ℃ of dry 2h (constant weight), and in exsiccator, being cooled to room temperature; Get respectively the spectroscopic pure lithium carbonate that 1.0000g is dry and treat test sample lithium carbonate sample, be placed in respectively reactor, in reactor, respectively add 90mL deionized water, under ultrasound wave is auxiliary by spectroscopic pure lithium carbonate with treat that test sample lithium carbonate sample dissolves respectively completely, then solution is transferred to respectively in 100mL volumetric flask, and is settled to 100mL; Respectively to the methyl orange indicator that drips 2 ~ 5 0.1%wt in the reactor that contains lithium carbonate solution, more respectively with the dilution heat of sulfuric acid of 0.05mol/L be titrated to faint yellow till; Calculate lithium carbonate content.For guaranteeing that accurately each sample is at least done three groups of parallel laboratory tests, and averages, and obtains lithium carbonate content.
In the present invention, employing methyl orange is indicator, and concentration is 0.1%wt left and right, generally drips 2-5 and drips, and adopts dilute sulfuric acid to carry out titration, and the concentration of dilute sulfuric acid is 0.05mol/L.
This method is applicable to lithium carbonate content in the detection of 90% sample, and testing result is more accurate, and this range detection error of low mistake is larger, does not advise adopting this method to detect.
Regulation (GB/T11064.1-2013) in national standard, while carrying out lithium carbonate content detection, the difference of two parallel analysis results in same experiment, should meet table 1 regulation, if outside tolerance, again detect again, do parallel laboratory test simultaneously, adopt this method to carry out a large amount of detection tests, the tolerance of gained all, within industry regulation, meets the demands.
Between table 1 laboratory, the difference of analysis result should be not more than the listed permissible value of following table
The present invention be take methyl orange as indicator, adopts dilute sulfuric acid titrimetry to replace original watery hydrochloric acid titrimetry, can be used for the mensuration of lithium carbonate content in sample.Compare with original method (watery hydrochloric acid titrimetry GB/T11064.1-2013), the present invention is simple to operate, and detection time is short, titration end-point is easy to judgement, has reduced error, is subject to the impact of the external conditions such as temperature, humidity little, agents useful for same toxicity is little, operation safe.
Embodiment
Below by specific embodiment, the present invention will be further elaborated.The lithium carbonate content of take is below example at more than 98% sample, by measuring lithium carbonate content in same sample, to comparing of original method (watery hydrochloric acid titration GB/T11064.1-2013) and detection method of the present invention.
The concrete operation method of lithium carbonate content in original working sample (watery hydrochloric acid titrimetry) is measured according to the experimental procedure in GB/T11064.1-2013 standard.
It is indicator that the present invention adopts methyl orange, and dilute sulfuric acid residual quantity titrimetry is carried out blank assay simultaneously, usings respectively and does not add the test of sample and do not add indicator as blank test.
It is indicator that the present invention adopts methyl orange, and dilute sulfuric acid residual quantity titrimetry is carried out 3 groups of parallel laboratory tests simultaneously, and concrete operation step comprises:
(1) get respectively 5.0000g spectroscopic pure lithium carbonate and treat test sample lithium carbonate sample, respectively at 300 ℃ of dry 2h (constant weight), and in exsiccator, being cooled to room temperature;
(2) get respectively the spectroscopic pure lithium carbonate that 1.0000g is dry and treat test sample lithium carbonate sample, being placed in respectively reactor, in reactor, respectively adding 90mL deionized water;
(3) under ultrasound wave is auxiliary by spectroscopic pure lithium carbonate with treat that test sample lithium carbonate sample dissolves respectively completely, is then transferred to solution respectively in 100mL volumetric flask, and is settled to 100mL;
(4) respectively to the methyl orange indicator that drips 2～5 0.1%wt in the reactor that contains lithium carbonate solution, then with the dilution heat of sulfuric acid of 0.05mol/L, to be titrated to faint yellow be respectively terminal, and the formula that is then calculated as follows is calculated lithium carbonate content.
The lithium carbonate content of two kinds of detection method tests is basically identical, and still, original method exists parallel laboratory test error large, CO in solution
2clearance is difficult to the defects such as judgement.
From method above, can find out, the present invention is simple to operate, and operate miss is little, and is subject to the extraneous factors such as temperature, humidity to affect less.
Claims (7)
1. a detection method for lithium carbonate content, is characterized in that the method comprises the following steps:
(1) take respectively the dry spectroscopic pure lithium carbonate of identical weight and treat in 250-350 ℃ of dry 2-3 h, and in exsiccator, to be cooled to room temperature by test sample lithium carbonate sample;
(2) respectively with deionized water by spectroscopic pure lithium carbonate and treat that test sample lithium carbonate sample dissolves completely;
(3) until spectroscopic pure lithium carbonate with after test sample lithium carbonate sample dissolves respectively completely, respectively to spectroscopic pure lithium carbonate solution with treat to add 2-5 to drip methyl orange indicator in test sample lithium carbonate sample solution, with dilute sulfuric acid be titrated to faint yellow till;
(4), after titration completes, be calculated as follows lithium carbonate content:
Lithium carbonate content=[0.9998 * M
spectroscopic pure sample-C
h2SO4* M
li2CO3* (V
h2SO4 spectroscopic pure sodium carbonate-V
h2SO4 treats test sample sodium carbonate)]/M
testing sample* 100%;
Wherein, spectroscopic pure lithium carbonate content is that 99.98%(demarcates), C
h2SO4for H
2sO
4amount of substance concentration, mol/L; V
h2SO4for the volume of dilute sulfuric acid that titration consumes, L; M
li2CO3for the molal weight of lithium carbonate, 73.89 g/mol; M
spectroscopic pure samplefor the quality of taken spectroscopic pure sample, the g of unit; M
testing samplefor the quality of taken sample to be measured, the g of unit.
2. according to the detection method of the lithium carbonate content described in claim 1, it is characterized in that: in step (1), spectroscopic pure lithium carbonate and treat test sample lithium carbonate sample, in 300 ℃ of dry 2 h.
3. according to the detection method of the lithium carbonate content described in claim 1, it is characterized in that: in step (2), adopt deionized water dissolving lithium carbonate sample, and use ultrasound wave assist in dissolving.
4. according to the detection method of the lithium carbonate content described in claim 1, it is characterized in that: in step (3), the concentration of dilute sulfuric acid is 0.01-0.20mol/L.
5. according to the detection method of the lithium carbonate content described in claim 1, it is characterized in that: treat in test sample lithium carbonate sample that lithium carbonate content is more than 90%.
6. according to the detection method of the lithium carbonate content described in claim 1, it is characterized in that: in step (1), get respectively 5.0000 g spectroscopic pure lithium carbonates and treat test sample lithium carbonate sample, respectively at 300 ℃ of dry 2 h, and in exsiccator, be cooled to room temperature; In step (2), get respectively the spectroscopic pure lithium carbonate that 1.0000 g are dry and treat test sample lithium carbonate sample, being placed in respectively reactor, in reactor, respectively adding 90 mL deionized waters; Under ultrasound wave is auxiliary by spectroscopic pure lithium carbonate with treat that test sample lithium carbonate sample dissolves respectively completely, is then transferred to solution respectively in 100 mL volumetric flasks, and is settled to 100 mL; In step (3), respectively to the methyl orange indicator that drips 2～5 0.1 % wt in the reactor that contains lithium carbonate solution, more respectively with the dilution heat of sulfuric acid of 0.05 mol/L be titrated to faint yellow till; Calculate lithium carbonate content.
7. according to the detection method of the lithium carbonate content described in claim 6, it is characterized in that: blank assay and titration experiments are done respectively three groups of parallel laboratory tests, and get its mean value.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053460A (en) * | 2016-07-20 | 2016-10-26 | 天津国安盟固利新材料科技股份有限公司 | Method for detecting lithium content in lithium battery cathode material mixture |
| CN106556670A (en) * | 2016-10-21 | 2017-04-05 | 多氟多（焦作）新能源科技有限公司 | A kind of detection method of tertiary cathode material surface lithium |
| CN108181428A (en) * | 2017-12-29 | 2018-06-19 | 南通瑞翔新材料有限公司 | A kind of detection method of boracic tertiary cathode material remnants alkali contents |
| CN111122548A (en) * | 2020-01-06 | 2020-05-08 | 江苏容汇通用锂业股份有限公司 | Method for detecting trace metal copper and zinc in lithium carbonate |
| CN111129486A (en) * | 2019-12-27 | 2020-05-08 | 中天新兴材料有限公司 | Method for preparing ternary cathode material of lithium battery |
| CN112067493A (en) * | 2020-09-16 | 2020-12-11 | 百杰瑞(荆门)新材料有限公司 | Water content detection method of anhydrous lithium iodide |
| CN114813616A (en) * | 2022-06-29 | 2022-07-29 | 四川富临新能源科技有限公司 | Device and method for detecting carbon content in lithium iron phosphate |
-
2014
- 2014-05-13 CN CN201410200406.4A patent/CN103954617B/en not_active Expired - Fee Related
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053460A (en) * | 2016-07-20 | 2016-10-26 | 天津国安盟固利新材料科技股份有限公司 | Method for detecting lithium content in lithium battery cathode material mixture |
| CN106556670A (en) * | 2016-10-21 | 2017-04-05 | 多氟多（焦作）新能源科技有限公司 | A kind of detection method of tertiary cathode material surface lithium |
| CN108181428A (en) * | 2017-12-29 | 2018-06-19 | 南通瑞翔新材料有限公司 | A kind of detection method of boracic tertiary cathode material remnants alkali contents |
| CN111129486A (en) * | 2019-12-27 | 2020-05-08 | 中天新兴材料有限公司 | Method for preparing ternary cathode material of lithium battery |
| CN111129486B (en) * | 2019-12-27 | 2021-05-14 | 中天新兴材料有限公司 | Method for preparing ternary cathode material of lithium battery |
| CN111122548A (en) * | 2020-01-06 | 2020-05-08 | 江苏容汇通用锂业股份有限公司 | Method for detecting trace metal copper and zinc in lithium carbonate |
| CN112067493A (en) * | 2020-09-16 | 2020-12-11 | 百杰瑞(荆门)新材料有限公司 | Water content detection method of anhydrous lithium iodide |
| CN114813616A (en) * | 2022-06-29 | 2022-07-29 | 四川富临新能源科技有限公司 | Device and method for detecting carbon content in lithium iron phosphate |
| CN114813616B (en) * | 2022-06-29 | 2022-11-08 | 四川富临新能源科技有限公司 | Device and method for detecting carbon content in lithium iron phosphate battery negative electrode material |
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