CN103954617B - Method for detecting content of lithium carbonate - Google Patents
Method for detecting content of lithium carbonate Download PDFInfo
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- CN103954617B CN103954617B CN201410200406.4A CN201410200406A CN103954617B CN 103954617 B CN103954617 B CN 103954617B CN 201410200406 A CN201410200406 A CN 201410200406A CN 103954617 B CN103954617 B CN 103954617B
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- lithium carbonate
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- carbonic acid
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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 is and in particular to a kind of detection method of carbonic acid lithium content.
Background technology
Lithium carbonate is the basic material producing lithium compound and lithium metal, is one of most important product in lithium industry.Carbonic acid
Lithium is widely used in the fields such as pottery, lithium battery, pharmacy, food, metal smelt.
With application in lithium battery for the lithium carbonate, the detection of high-purity lithium carbonate product is more and more important.Existing detection
The method of carbonic acid lithium content is " hydrochloric titration ", and using C.I. 13020 .-bromocresol green as indicator, Lithium carbonate solution is through dilute hydrochloric acid
Titration, forms lithium chloride, by measuring the consumption of dilute hydrochloric acid, calculates the carbonic acid lithium content in testing sample.The method exists drips
Determine terminal to be difficult to judge, in solution, the carbon dioxide of residual will make titration error amplify, and titration results are subject to temperature, humidity
The defect such as big etc. external condition impact.Time-consuming, personal error big for the method presence, big by ectocine, is unfavorable for high accuracy
And quick detection.
Content of the invention
Not enough present in existing lithium carbonate detection method of content in order to overcome, it is an object of the invention to provide a kind of carbonic acid
The detection method of lithium content, this method is simple to operate, low cost, time-consuming few, and detection efficiency is high, by external worlds such as temperature, humidity
Condition impact is little.
The purpose of the present invention is achieved through the following technical solutions:
A kind of detection method of carbonic acid lithium content is it is characterised in that the method comprises the following steps:
(1) weigh the dry spectroscopic pure lithium carbonate of identical weight respectively and treat test sample lithium carbonate sample, in 250-350 DEG C
2-3h (constant weight) is dried, and is cooled to room temperature in exsiccator；
(2) deionized water by spectroscopic pure lithium carbonate and treats that test sample lithium carbonate sample is completely dissolved respectively；
(3) after spectroscopic pure lithium carbonate with after test sample lithium carbonate sample is completely dissolved respectively, respectively to spectroscopic pure lithium carbonate
Solution and treat in test sample lithium carbonate sample solution add 2-5 drip methyl orange indicator, with dilute sulfuric acid be titrated to faint yellow till；
(4), after the completion of titrating, it is calculated as follows carbonic acid lithium content:
Carbonic acid lithium content=[0.9998 × mSpectroscopic pure sample-ch2so4×mli2co3×(vH2so4 spectroscopic pure lithium carbonate-vH2so4 treats test sample lithium carbonate)]/
mTesting sample× 100%；
Wherein, spectroscopic pure carbonic acid lithium content is 99.98% (demarcating), ch2so4For h2so4Substance withdrawl syndrome, mol/
l；vh2so4By titration consumption dilute sulfuric acid volume, l；mli2co3For the molal weight of lithium carbonate, 73.89g/mol；mSpectroscopic pure sampleFor
The quality of weighed spectroscopic pure sample, g；mTesting sampleBy the quality of weighed sample to be measured, g.
In the present invention, under ultrasonic assistant, using deionized water dissolving lithium carbonate sample.The concentration of dilute sulfuric acid is
0.01-0.20mol/l.Treat that in test sample lithium carbonate sample, carbonic acid lithium content is more than 90%.
In the present invention, preferred detecting step is: takes 5.0000g spectroscopic pure lithium carbonate respectively and treats test sample lithium carbonate sample
Product, are dried 2h (constant weight) respectively at 300 DEG C, and are cooled to room temperature in exsiccator；Take the dry spectroscopic pure of 1.0000g respectively
Lithium carbonate and treat test sample lithium carbonate sample, is respectively placed in reactor, each in reactor adds 90ml deionized water, in ultrasound wave
By spectroscopic pure lithium carbonate and treat that test sample lithium carbonate sample is completely dissolved respectively under auxiliary, then solution is transferred to respectively 100ml
In volumetric flask, and it is settled to 100ml；Respectively to the methyl of 2～5 0.1%wt of Deca in the reactor containing Lithium carbonate solution
Orange indicator, more respectively with the dilution heat of sulfuric acid of 0.05mol/l be titrated to faint yellow till；Calculate carbonic acid lithium content.For ensureing
Accurately, each sample at least does three groups of parallel laboratory tests, and averages, and obtains carbonic acid lithium content.
In the present invention, it is indicator using methyl orange, concentration is 0.1%wt, and general Deca 2-5 is dripped, using dilute sulfur
Acid is titrated, and the concentration of dilute sulfuric acid is 0.05mol/l.
This method is applied to the detection in 90% sample for the carbonic acid lithium content, and testing result is more accurate, this range detection of low mistake
Error larger it is not recommended that being detected using this method.
Specify (gb/t 11064.1-2013), when carrying out lithium carbonate content detection, two in same experiment in national standard
The difference of parallel analysis result, should meet table 1 and specify, if outside tolerance, again will detect again, do parallel reality simultaneously
Test, substantial amounts of detection test has been carried out using this method, the tolerance of gained, all within industry regulation, meets and requires.
Between table 1 laboratory, the difference of analysis result should be not more than permissible value listed in Table
The present invention, with methyl orange as indicator, replaces original dilute hydrochloric acid titrimetry using dilute sulfuric acid titrimetry, can be used for sample
The mensure of carbonic acid lithium content in product.Compared with original method (dilute hydrochloric acid titrimetry gb/t 11064.1-2013), the present invention operates
Simply, detection time is short, and titration end-point is easy to judge, reduces error, is affected little, institute by external conditions such as temperature, humidity
Little with reagent toxicity, operation is safer.
Specific embodiment
Below by specific embodiment, the present invention will be further elaborated.Below with carbonic acid lithium content more than 98%
Sample as a example, by measure same sample in carbonic acid lithium content, to original method (dilute hydrochloric acid titrate gb/t 11064.1-
2013) and the comparing of detection method.
In original determination sample, the concrete operation method (dilute hydrochloric acid titrimetry) of carbonic acid lithium content is according to gb/t 11064.1-
Experimental procedure in 2013 standards is measured.
It is indicator that the present invention adopts methyl orange, and dilute sulfuric acid residual quantity titrimetry carries out blank experiment simultaneously, respectively not add
The test of sample and plus indicator as blank assay.
It is indicator that the present invention adopts methyl orange, and dilute sulfuric acid residual quantity titrimetry carries out 3 groups of parallel laboratory tests simultaneously, concrete behaviour
Include as step:
(1) take 5.0000g spectroscopic pure lithium carbonate respectively and treat test sample lithium carbonate sample, 2h is dried respectively at 300 DEG C (permanent
Weight), and it is cooled to room temperature in exsiccator；
(2) take the dry spectroscopic pure lithium carbonate of 1.0000g respectively and treat test sample lithium carbonate sample, be respectively placed in reactor
In, each addition 90ml deionized water in reactor；
(3) by spectroscopic pure lithium carbonate and treat that test sample lithium carbonate sample is completely dissolved respectively under ultrasonic assistant, then will
Solution is transferred in 100ml volumetric flask respectively, and is settled to 100ml；
(4) respectively to the methyl orange indicator of 2～5 0.1%wt of Deca in the reactor containing Lithium carbonate solution, then divide
Not with the dilution heat of sulfuric acid of 0.05mol/l be titrated to faint yellow for terminal, the formula that is then calculated as follows calculates carbonic acid lithium content.
Carbonic acid lithium content=[0.9998 × 1.0000-0.05 × 73.89 × (vH2so4 spectroscopic pure lithium carbonate-vH2so4 treats test sample lithium carbonate)]/
1.0000 × 100%.
The carbonic acid lithium content of two kinds of detection method tests is basically identical, but, there is parallel laboratory test error greatly in original method,
Co in solution2Clearance is difficult to the defects such as judgement.
From above method as can be seen that the present invention is simple to operate, operating error is little, and by temperature, humidity etc. extraneous because
Element impact is less.
Claims (6)
1. a kind of detection method of carbonic acid lithium content is it is characterised in that the method comprises the following steps:
(1) weigh the dry spectroscopic pure lithium carbonate of identical weight respectively and treat test sample lithium carbonate sample, in 250-350 DEG C of drying
2-3h, and it is cooled to room temperature in exsiccator；Treat that in test sample lithium carbonate sample, carbonic acid lithium content is more than 98%；
(2) deionized water by spectroscopic pure lithium carbonate and treats that test sample lithium carbonate sample is completely dissolved respectively；
(3) after spectroscopic pure lithium carbonate with after test sample lithium carbonate sample is completely dissolved respectively, respectively to spectroscopic pure Lithium carbonate solution
With treat in test sample lithium carbonate sample solution add 2-5 drip methyl orange indicator, with dilute sulfuric acid be titrated to faint yellow till；
(4), after the completion of titrating, it is calculated as follows carbonic acid lithium content:
Carbonic acid lithium content=[0.9998 × mSpectroscopic pure sample-ch2so4×mli2co3×(vH2so4 spectroscopic pure lithium carbonate-vH2so4 treats test sample lithium carbonate)]/mTesting sample
× 100%；
Wherein, spectroscopic pure carbonic acid lithium content is 99.98%, and this spectroscopic pure lithium carbonate is demarcated, ch2so4For h2so4Material amount
Concentration, mol/l；vh2so4By titration consumption dilute sulfuric acid volume, l；mli2co3For the molal weight of lithium carbonate, 73.89g/mol；
mSpectroscopic pure sampleBy the quality of weighed spectroscopic pure sample, g；mTesting sampleBy the quality of weighed sample to be measured, g.
2. carbonic acid lithium content according to claim 1 detection method it is characterised in that: in step (1), spectroscopic pure carbonic acid
Lithium and treat test sample lithium carbonate sample, is dried 2h in 300 DEG C.
3. carbonic acid lithium content according to claim 1 detection method it is characterised in that: in step (2), using deionization
Water dissolution lithium carbonate sample, and dissolved with ultrasonic assistant.
4. carbonic acid lithium content according to claim 1 detection method it is characterised in that: in step (3), dilute sulfuric acid dense
Spend for 0.01-0.20mol/l.
5. carbonic acid lithium content according to claim 1 detection method it is characterised in that: in step (1), take respectively
5.0000g spectroscopic pure lithium carbonate and treat test sample lithium carbonate sample, is dried 2h respectively at 300 DEG C, and is cooled to room in exsiccator
Temperature；In step (2), take the dry spectroscopic pure lithium carbonate of 1.0000g respectively and treat test sample lithium carbonate sample, be respectively placed in reaction
In device, each addition 90ml deionized water in reactor；By spectroscopic pure lithium carbonate and treat test sample lithium carbonate sample under ultrasonic assistant
Product are completely dissolved respectively, then solution are transferred in 100ml volumetric flask respectively, and are settled to 100ml；In step (3), respectively
The methyl orange indicator of 2～5 0.1%wt of Deca in the reactor containing Lithium carbonate solution, then use 0.05mol/l's respectively
Dilution heat of sulfuric acid be titrated to faint yellow till；Calculate carbonic acid lithium content.
6. carbonic acid lithium content according to claim 5 detection method it is characterised in that: blank experiment and titration experiments are divided
Do not do three groups of parallel laboratory tests, and take its meansigma methods.
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| 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 |
| 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 |
| 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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| 井卤生产碳酸锂中碳酸锂的快速测定;张进棠等;《中国井矿盐》;19981231(第2期);全文 * |
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Effective date of registration: 20170919 Address after: 221000 Jiangsu city of Xuzhou province Peixian Huxi farm gate No. 389 Patentee after: Shen Zhaohai Address before: 210016 Jiangsu Province, Nanjing Xianlin University City, Yang Shan Road No. 1 Patentee before: Nanjing Institute of Industry Technology |
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