CN111122548A - Method for detecting trace metal copper and zinc in lithium carbonate - Google Patents
Method for detecting trace metal copper and zinc in lithium carbonate Download PDFInfo
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- CN111122548A CN111122548A CN202010009236.7A CN202010009236A CN111122548A CN 111122548 A CN111122548 A CN 111122548A CN 202010009236 A CN202010009236 A CN 202010009236A CN 111122548 A CN111122548 A CN 111122548A
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 69
- 239000011701 zinc Substances 0.000 title claims abstract description 69
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 68
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 68
- 239000010949 copper Substances 0.000 title claims abstract description 68
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 38
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910021654 trace metal Inorganic materials 0.000 title claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 7
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 3
- 239000012982 microporous membrane Substances 0.000 claims abstract 3
- 239000000243 solution Substances 0.000 claims description 45
- 238000005406 washing Methods 0.000 claims description 18
- 238000002835 absorbance Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000012086 standard solution Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims 2
- QUQFTIVBFKLPCL-UHFFFAOYSA-L copper;2-amino-3-[(2-amino-2-carboxylatoethyl)disulfanyl]propanoate Chemical compound [Cu+2].[O-]C(=O)C(N)CSSCC(N)C([O-])=O QUQFTIVBFKLPCL-UHFFFAOYSA-L 0.000 claims 1
- 238000005374 membrane filtration Methods 0.000 claims 1
- 230000020477 pH reduction Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- -1 zinc metals Chemical class 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明公开了一种碳酸锂中微量金属铜、锌的检测方法，包含以下步骤；称取100‑250克的碳酸锂加水调成浆料，通入二氧化碳气体，使其完全溶解成为碳化液；将微孔滤膜固定在杯式过滤器上，连接杯式过滤器和真空泵，采用微孔滤膜对碳化液进行过滤，使得碳化液中的金属单质留在滤膜上；将微孔滤膜采用氨水或硝酸处理，使微孔滤膜上的金属铜、锌溶解；将铜、锌溶解后得到的溶液加热至近干，然后转移至容量瓶中定容；采用等离子体原子发射光谱对溶液中的铜、锌进行测定,本发明检测结果较为准确可靠，处理后的溶液可直接返回生产线，不会造成物料的浪费,本发明适用于粉碎过的工业级碳酸锂、电池级碳酸锂、高纯碳酸锂中金属铜、锌的测定。
The invention discloses a method for detecting trace metal copper and zinc in lithium carbonate, comprising the following steps: weighing 100-250 grams of lithium carbonate and adding water to prepare a slurry, and introducing carbon dioxide gas to completely dissolve it into a carbonized liquid; Fix the microporous filter membrane on the cup filter, connect the cup filter and the vacuum pump, use the microporous filter membrane to filter the carbonized liquid, so that the metal element in the carbonized liquid remains on the filter membrane; the microporous filter membrane Treat with ammonia or nitric acid to dissolve metal copper and zinc on the microporous membrane; heat the solution obtained by dissolving copper and zinc to near dryness, and then transfer it to a volumetric flask for constant volume; The detection results of the present invention are more accurate and reliable, and the treated solution can be directly returned to the production line without causing waste of materials. The present invention is suitable for pulverized industrial grade lithium carbonate, battery grade lithium carbonate, high-purity Determination of metallic copper and zinc in lithium carbonate.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for detecting trace metal copper and zinc in lithium carbonate.
Background
In recent years, with the improvement of a system for evaluating the safety of battery materials, the requirement of the content of impurities in lithium carbonate is higher. Among the factors affecting the safety performance of the battery, in addition to the problems of electrolyte, pole piece, diaphragm, etc. previously recognized by scientists, metal impurities in the battery material also cause overcharge of the battery, lead to poor storage performance, affect the consistency of the battery, and even cause local short circuit inside the battery, thereby causing self-discharge and safety accidents, which has gradually become a consensus of most battery manufacturers. Therefore, manufacturers who produce battery materials monitor the entire production process for foreign matter.
The source of metal copper and zinc in lithium carbonate may be an environmental factor, and may also be the abrasion introduction of equipment related to the production process, the content is low, trace metal copper and zinc existing in a metal state in the lithium carbonate cannot be effectively detected by adopting a conventional acid treatment method, and a detection method for metal copper and zinc simple substances in lithium carbonate is not disclosed at present.
Disclosure of Invention
The invention aims to provide a method for detecting trace metal copper and zinc in lithium carbonate.
The technical scheme adopted by the invention is as follows:
a method for detecting trace metals of copper and zinc in lithium carbonate is characterized by comprising the following steps: comprises the following steps;
step 1: weighing 100-250 g of lithium carbonate, adding water to prepare slurry, and introducing carbon dioxide gas to completely dissolve the slurry to obtain a carbonized liquid;
step 2: fixing a microporous filter membrane on a cup-type filter, connecting the cup-type filter with a vacuum pump, and filtering the carbonized liquid by adopting the microporous filter membrane to ensure that the metal simple substance in the carbonized liquid is remained on the filter membrane;
and step 3: treating the microporous filter membrane by ammonia water or nitric acid to dissolve metal copper and zinc on the microporous filter membrane;
and 4, step 4: heating the solution obtained after dissolving copper and zinc to be nearly dry, and then transferring the solution to a volumetric flask for constant volume;
and 5: and (3) measuring the copper and the zinc in the solution by adopting plasma atomic emission spectroscopy.
In the step 1, the solid content of the slurry is 20-40%.
In the step 2, when the carbonized liquid is filtered, the carbonized liquid is poured into a cup type filter, suction filtration is carried out, all filtrate passes through the filter membrane, and the filter membrane is washed by pure water for 2-5 times.
In the step 3, the specific steps of treating the microporous filter membrane by ammonia water or nitric acid are as follows: taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a beaker, adding ammonia water with the volume concentration of 20-80% or 10ml of concentrated nitric acid, heating at low temperature for 5-20min, cooling, filtering on the cup filter by using the microporous filter membrane, washing the filter membrane for 3-6 times by using 90-110ml of water, and collecting filtrate and washing water to obtain a solution with dissolved copper and zinc.
In the step 4, the solution is heated to be nearly dry and then is acidified by nitric acid, and the acidity of the solution is controlled to be 5-10%.
In the step 5, the specific steps for measurement are as follows: respectively taking 0, 0.5, 1.0, 2.0, 5.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10ug/mL into a 100mL volumetric flask, adding 10mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on a plasma atomic emission spectrometer by taking water as a reference, drawing a standard curve, measuring the absorbance values of copper and zinc in the solution on the plasma atomic emission spectrometer by taking water as a reference, and checking the concentrations of copper and zinc on the standard curve.
The cup filter is a glass sand core suction filter and comprises a suction bottle at the bottom, a sand core joint is arranged on the suction bottle, a microporous filter membrane is arranged in a sand core at the top of the sand core joint, and a clamp is arranged on the side surface of the sand core joint for fixing.
The invention has the advantages that: the method for measuring the trace metal copper and zinc in the lithium carbonate adopts the steps of introducing carbon dioxide to dissolve the lithium carbonate, filtering the carbonized solution through a microporous filter membrane to enable metal simple substances in the solution to be left on the filter membrane, then utilizing ammonia water or nitric acid to dissolve or dissolve the metal copper and zinc on the microporous filter membrane, enabling the metal copper and zinc on the filter membrane to enter the solution, and measuring the copper and zinc in the solution by adopting a plasma spectrum after treatment to obtain the content of the metal copper and zinc in the solution. The method has simple process, can effectively detect trace metal copper and zinc in the lithium carbonate, has more accurate and reliable detection result, and can directly return the treated solution to a production line without causing material waste. The method is suitable for measuring the metal copper and zinc in the crushed industrial-grade lithium carbonate, the battery-grade lithium carbonate and the high-purity lithium carbonate.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic view of a cup filter of the present invention.
Wherein: 1. a suction flask; 2. A sand core joint; 3. a sand core; 4. a microporous filtration membrane; 5. and (4) a clamp.
Detailed Description
Example 1:
as shown in fig. 1, 200g of lithium carbonate was placed in a 10L clean plastic beaker, 7L of pure water was measured and poured into the beaker, and carbon dioxide was introduced into the beaker with continuous stirring to completely dissolve the lithium carbonate, and the solution was clear.
Fixing a water system microporous filter membrane 4 with the diameter of 50mm and the pore diameter of 0.8um on a cup type filter, connecting the cup type filter and a vacuum pump, turning on a switch of the vacuum pump, washing the filter membrane by 50mL of pure water, pouring the dissolved solution into the cup type filter, performing suction filtration, enabling all filtrate to pass through the filter membrane, washing the wall of the beaker by the pure water for 5 times, and washing the filter membrane for 5 times.
And taking the microporous filter membrane 4 off the cup filter, putting the microporous filter membrane into a 250mL beaker, adding ammonia water with the volume concentration of 40%, heating at low temperature for 20min to dissolve the metal copper and zinc on the microporous filter membrane, cooling, filtering the microporous filter membrane by using a 0.45-micrometer microporous filter membrane, washing the filter membrane for 3 times by using a small amount of water, collecting filtrate and washing water to obtain a solution with the dissolved copper and zinc, and transferring the solution into the 250mL beaker.
Heating the solution obtained after dissolving copper and zinc in the beaker to enable ammonia in the beaker to overflow until the volume is less than or equal to 10mL, slightly cooling, adding nitric acid, controlling the acidity of the solution to be 10%, heating and dissolving for 10min, cooling, and then transferring into a 100mL volumetric flask for constant volume.
And (3) measuring copper and zinc in the solution by adopting plasma spectroscopy: respectively putting 0mL of copper and zinc standard solution with the concentration of 10ug/mL, 0.5 mL, 1.0 mL, 2.0 mL, 5.0 mL and 10.0mL into a 100mL volumetric flask, adding 10mL of nitric acid into the volumetric flask, fixing the volume by using water, measuring the absorbance values of the copper and the zinc on a plasma atomic emission spectrometer by using the water as a reference, and automatically drawing a standard curve by an instrument; on a plasma atomic emission spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the contents of copper and zinc are found out on a standard curve.
Table 1: in example 1, the same lithium carbonate sample was subjected to 11 measurements to obtain metal copper and zinc contents (ppb)
Example 2:
as shown in fig. 1, 150g of lithium carbonate was placed in a 10L clean plastic beaker, 5L of pure water was measured and poured into the beaker, and carbon dioxide was introduced into the beaker with continuous stirring to completely dissolve the lithium carbonate, and the solution was clear.
Fixing a water system microporous filter membrane 4 with the diameter of 50mm and the pore diameter of 0.8um on a cup type filter, connecting the cup type filter and a vacuum pump, turning on a switch of the vacuum pump, washing the filter membrane by 50mL of pure water, pouring the dissolved solution into the cup type filter, performing suction filtration, enabling all filtrate to pass through the filter membrane, washing the wall of the beaker by the pure water for 5 times, and washing the filter membrane for 5 times.
And (3) taking the microporous filter membrane 4 off the cup filter, putting the microporous filter membrane into a 250mL beaker, adding 10mL nitric acid, heating at a low temperature for 10min to dissolve the copper and zinc metals on the microporous filter membrane, cooling, filtering the microporous filter membrane on the cup filter by using the 0.45um microporous filter membrane 4, washing the filter membrane for 3 times by using a small amount of water, collecting filtrate and washing water to obtain a solution with the dissolved copper and zinc, and transferring the solution into the 250mL beaker.
And heating the solution obtained after the copper and the zinc are dissolved in the beaker until the volume is less than or equal to 10mL, cooling, and transferring the solution into a 100mL volumetric flask for constant volume.
And (3) measuring copper and zinc in the solution by adopting plasma spectroscopy: respectively putting 0mL of copper and zinc standard solution with the concentration of 10ug/mL, 0.5 mL, 1.0 mL, 2.0 mL, 5.0 mL and 10.0mL into a 100mL volumetric flask, adding 10mL of nitric acid into the volumetric flask, fixing the volume by using water, measuring the absorbance values of the copper and the zinc on a plasma atomic emission spectrometer by using the water as a reference, and automatically drawing a standard curve by an instrument; on a plasma atomic emission spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the contents of copper and zinc are found out on a standard curve.
Table 2: in example 2, the same lithium carbonate sample was subjected to 11 measurements to obtain metal copper and zinc contents (ppb)
Example 3:
as shown in FIG. 1, 100g of lithium carbonate was placed in a 5L clean plastic beaker, and 4L of purified water was measured and poured into the beaker. And introducing carbon dioxide into the beaker and continuously stirring to completely dissolve the lithium carbonate, so that the solution is clear.
Fixing a water system microporous filter membrane with the diameter of 50mm and the pore diameter of 0.8um on a cup type filter, connecting the cup type filter and a vacuum pump, turning on a switch of the vacuum pump, washing the filter membrane by 50mL of pure water, pouring the dissolved solution into the cup type filter, performing suction filtration, enabling all filtrate to pass through the filter membrane, washing the wall of the beaker by the pure water for 5 times, and washing the filter membrane for 5 times.
And taking the microporous filter membrane 4 off the cup filter, putting the microporous filter membrane into a 250mL beaker, adding 5mL nitric acid, heating at a low temperature for 10min to dissolve the metallic copper and zinc on the microporous filter membrane, cooling, filtering the microporous filter membrane on the cup filter by using the 0.45um microporous filter membrane 4, washing the microporous filter membrane for 3 times by using a small amount of water, collecting filtrate and washing water to obtain a solution with the dissolved copper and zinc, and transferring the solution into the 250mL beaker.
And heating the solution obtained after the copper and the zinc are dissolved in the beaker until the volume is less than or equal to 10mL, cooling, and transferring the solution into a 100mL volumetric flask for constant volume.
And (3) measuring copper and zinc in the solution by adopting plasma spectroscopy: respectively putting 0mL of copper and zinc standard solution with the concentration of 10ug/mL, 0.5 mL, 1.0 mL, 2.0 mL, 5.0 mL and 10.0mL into a 100mL volumetric flask, adding 5mL of nitric acid into the volumetric flask, fixing the volume by using water, measuring the absorbance values of the copper and the zinc on a plasma atomic emission spectrometer by using water as reference, and automatically drawing a standard curve by an instrument; on a plasma atomic emission spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the contents of copper and zinc are found out on a standard curve.
Table 3: in example 3, the same lithium carbonate sample was subjected to 11 measurements to obtain the contents of metallic copper and zinc. (ppb)
Claims (7)
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| CN202010009236.7A CN111122548A (en) | 2020-01-06 | 2020-01-06 | Method for detecting trace metal copper and zinc in lithium carbonate |
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| CN202010009236.7A CN111122548A (en) | 2020-01-06 | 2020-01-06 | Method for detecting trace metal copper and zinc in lithium carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114308372A (en) * | 2021-12-16 | 2022-04-12 | 江西师范大学 | A kind of separation and waste liquid recovery method of microplastics in soil or sediment |
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