CN109883971B - Method for measuring trace metal copper and zinc in nickel-cobalt solution - Google Patents
Method for measuring trace metal copper and zinc in nickel-cobalt solution Download PDFInfo
- Publication number
- CN109883971B CN109883971B CN201910214304.0A CN201910214304A CN109883971B CN 109883971 B CN109883971 B CN 109883971B CN 201910214304 A CN201910214304 A CN 201910214304A CN 109883971 B CN109883971 B CN 109883971B
- Authority
- CN
- China
- Prior art keywords
- zinc
- solution
- filter membrane
- copper
- nickel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring trace metal copper and zinc in a nickel-cobalt solution, which comprises the steps of filtering the nickel-cobalt solution by using a microporous filter membrane, enabling a metal simple substance in the nickel-cobalt solution to remain on the filter membrane, then selectively dissolving the metal copper, zinc or an alloy thereof on the microporous filter membrane by using ammonia water, enabling the metal copper and zinc on the filter membrane to enter the solution, measuring the copper and zinc in the solution by using an atomic absorption spectrum or a plasma spectrum after treatment, and obtaining the content of the metal copper and zinc in the solution. The method has simple process, can effectively detect trace metals of copper and zinc in the solution, has 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 trace metal copper and zinc in nickel sulfate, cobalt chloride, cobalt nitrate, cobalt sulfate and nickel-cobalt mixed solution or mixed solution mainly containing nickel and cobalt and other metals.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for measuring trace metal copper and zinc in a nickel-cobalt solution for a battery material.
Background
The nickel solution can be used for preparing salt materials such as nickel sulfate or nickel hydroxide and the like, and can also be used for preparing ternary oxides such as nickel cobalt manganese, nickel cobalt aluminum and the like, the cobalt solution can be used for preparing ternary oxides of cobaltosic oxide or cobalt, the materials can be used for preparing nickel-hydrogen batteries or lithium ion batteries, the nickel-hydrogen batteries or the lithium ion batteries have high requirements on metal foreign matters such as silver, copper, zinc and the like, and safety accidents can be caused when the content of the foreign matters exceeds the range, so foreign matters can be monitored in the whole production process by a company for producing battery materials, including the nickel solution and the cobalt solution. The influence of metal foreign matters on a battery manufacturer depends not only on the content of the foreign matters but also on the size of the foreign matters, and generally, foreign matters with the size of more than 0.8um are harmful.
The sources of the metal copper and zinc in the nickel and cobalt solution can be environmental factors and can also be the abrasion introduction of relevant equipment in the production process, the content is low, and trace metal copper and zinc existing in a metal state in the nickel and cobalt solution cannot be effectively detected by adopting a conventional acid treatment method.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides the method for measuring the trace metal copper and zinc in the nickel-cobalt solution, which has simple process, can effectively detect the trace metal copper and zinc and has accurate detection result.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for measuring trace metals of copper and zinc in a nickel-cobalt solution comprises the following steps:
A. fixing the microporous filter membrane on a cup-type filter, connecting the filter with a vacuum pump, turning on a switch of the vacuum pump, and washing the filter membrane with pure water;
B. filtering the nickel-cobalt solution by adopting a microporous filter membrane to ensure that the metal simple substance in the nickel-cobalt solution is remained on the filter membrane;
C. treating the microporous filter membrane by ammonia water to dissolve metal copper and zinc on the microporous filter membrane;
D. heating and evaporating a solution obtained after copper and zinc are dissolved to dryness, and acidifying after evaporation to dryness, wherein the acidity of the solution is controlled to be 2-5%;
E. and measuring the copper and the zinc in the solution by adopting an atomic absorption spectrum or a plasma spectrum.
And further, when filtering the nickel-cobalt solution in the step B, pouring the nickel-cobalt solution into a cup filter, carrying out suction filtration, enabling all filtrate to pass through the filter membrane, and washing the filter membrane for 2-5 times by using pure water.
Further, the step C of treating the microporous filter membrane with ammonia water comprises the following specific steps: taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a container, adding ammonia water with the volume concentration of 20-80%, 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 a small amount of water, and collecting filtrate and washing water to obtain a solution in which copper and zinc are dissolved.
Further, the specific steps of step D are: heating the solution obtained after dissolving copper and zinc to overflow ammonia until the volume is less than or equal to 5mL, slightly cooling, adding nitric acid (1 + 1), controlling the acidity of the solution to be 2-5%, heating and dissolving for 2-20min, cooling, and transferring into a volumetric flask to fix the volume.
Further, the specific steps of the measurement in the step E are as follows: respectively putting 0, 2.0, 4.0, 8.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10ug/mL into a 100mL volumetric flask, adding 2mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on an atomic absorption spectrometer or a plasma spectrometer by taking water as a reference, and automatically drawing a standard curve by an instrument; on an atomic absorption spectrometer or a plasma spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the concentrations of the copper and the zinc are checked on a standard curve.
Compared with the prior art, the invention has the following beneficial effects: the method for measuring the trace metal copper and zinc in the nickel-cobalt solution adopts a microporous filter membrane to filter the nickel-cobalt solution, so that a metal simple substance in the nickel-cobalt solution is left on the filter membrane, then ammonia water is used for selectively dissolving the metal copper, zinc or an alloy thereof on the microporous filter membrane, so that the metal copper and zinc on the filter membrane enter the solution, and after treatment, the atomic absorption spectrum or the plasma spectrum is adopted to measure the copper and zinc in the solution, so that the content of the metal copper and zinc in the solution is obtained. The method has simple process, can effectively detect trace metals of copper and zinc in the solution, has 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 trace metal copper and zinc in nickel sulfate, cobalt chloride, cobalt nitrate, cobalt sulfate and nickel-cobalt mixed solution or mixed solution mainly containing nickel and cobalt and other metals.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A. 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 filter and a vacuum pump, turning on a switch of the vacuum pump, and washing the filter membrane by 50mL of pure water.
B. Pouring 500mL of cobalt nitrate solution into a cup filter, carrying out suction filtration, enabling all filtrate to pass through the filter membrane, washing the filter membrane for 2 times by pure water, and using 10mL of water each time, so as to enable metal simple substances in the cobalt nitrate solution to be remained on the filter membrane.
C. And taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a 200mL beaker, adding ammonia water with the volume concentration of 20%, heating at low temperature for 5min 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 200mL beaker.
D. 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 5mL, slightly cooling, adding nitric acid (1 + 1), controlling the acidity of the solution to be 2%, heating and dissolving for 10min, cooling, and transferring into a volumetric flask to fix the volume.
E. And (3) measuring copper and zinc in the solution by adopting an atomic absorption spectrum or a plasma spectrum: respectively putting 0, 2.0, 4.0, 8.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10ug/mL into a 100mL volumetric flask, adding 2mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on an atomic absorption spectrometer or a plasma spectrometer by taking water as a reference, and automatically drawing a standard curve by an instrument; on an atomic absorption spectrometer or a plasma spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the concentrations of the copper and the zinc are checked on a standard curve.
Example 2
A. Fixing a water system microporous filter membrane with the diameter of 47mm and the pore diameter of 1.0um on a cup type filter, connecting the filter and a vacuum pump, turning on a switch of the vacuum pump, and washing the filter membrane by 50mL of pure water.
B. Pouring 1000mL of nickel sulfate solution into a cup filter, carrying out suction filtration, enabling all filtrate to pass through the filter membrane, washing the filter membrane for 5 times by pure water, and using 10mL of water each time, so that the metal simple substance in the nickel sulfate solution is remained on the filter membrane.
C. Taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a 200mL beaker, adding ammonia water with the volume concentration of 80%, heating at low temperature for 20min to dissolve the metal copper and zinc on the microporous filter membrane, cooling, filtering the microporous filter membrane with a 0.30-micrometer microporous filter membrane on the cup filter, washing the filter membrane with a small amount of water for 6 times, collecting filtrate and washing water to obtain a solution with the dissolved copper and zinc, and transferring the solution into the 200mL beaker.
D. 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 5mL, slightly cooling, adding nitric acid (1 + 1), controlling the acidity of the solution to be 5%, heating and dissolving for 20min, cooling, and transferring into a volumetric flask to fix the volume.
E. And (3) measuring copper and zinc in the solution by adopting an atomic absorption spectrum or a plasma spectrum: respectively putting 0, 2.0, 4.0, 8.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10ug/mL into a 100mL volumetric flask, adding 2mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on an atomic absorption spectrometer or a plasma spectrometer by taking water as a reference, and automatically drawing a standard curve by an instrument; on an atomic absorption spectrometer or a plasma spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the concentrations of the copper and the zinc are checked on a standard curve.
Example 3
A. Fixing a water system microporous filter membrane with the diameter of 50mm and the pore diameter of 1.0um on a cup type filter, connecting the filter and a vacuum pump, turning on a switch of the vacuum pump, and washing the filter membrane by 50mL of pure water.
B. And pouring 2000mL of the mixed solution of nickel sulfate and cobalt sulfate into a cup filter, carrying out suction filtration, enabling all filtrate to pass through the filter membrane, washing the filter membrane for 3 times by pure water, and using 10mL of water each time, so that the metal simple substance in the mixed solution of nickel sulfate and cobalt sulfate is remained on the filter membrane.
C. Taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a 200mL beaker, adding ammonia water with the volume concentration of 50%, heating at low temperature for 10min to dissolve the metal copper and zinc on the microporous filter membrane, cooling, filtering the microporous filter membrane with a 0.30-micrometer microporous filter membrane on the cup filter, washing the filter membrane with a small amount of water for 5 times, collecting filtrate and washing water to obtain a solution with the dissolved copper and zinc, and transferring the solution into the 200mL beaker.
D. 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 5mL, slightly cooling, adding nitric acid (1 + 1), controlling the acidity of the solution to be 3%, heating and dissolving for 2min, cooling, and transferring into a volumetric flask to fix the volume.
E. And (3) measuring copper and zinc in the solution by adopting an atomic absorption spectrum or a plasma spectrum: respectively putting 0, 2.0, 4.0, 8.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10ug/mL into a 100mL volumetric flask, adding 2mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on an atomic absorption spectrometer or a plasma spectrometer by taking water as a reference, and automatically drawing a standard curve by an instrument; on an atomic absorption spectrometer or a plasma spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the concentrations of the copper and the zinc are checked on a standard curve.
The measurement conditions of the atomic absorption spectrometry and the plasma spectrometry in the above examples are shown in tables 1 and 2:
TABLE 1 determination conditions by atomic absorption spectrometry
TABLE 2 plasma Spectroscopy determination method
Claims (2)
1. A method for measuring trace metals of copper and zinc in a nickel-cobalt solution is characterized by comprising the following steps:
A. fixing the microporous filter membrane on a cup-type filter, connecting the filter with a vacuum pump, turning on a switch of the vacuum pump, and washing the filter membrane with pure water;
B. filtering the nickel-cobalt solution by adopting a microporous filter membrane to ensure that the metal simple substance in the nickel-cobalt solution is remained on the filter membrane;
C. treating the microporous filter membrane by ammonia water to dissolve metal copper and zinc on the microporous filter membrane; the method comprises the following specific steps of treating the microporous filter membrane by ammonia water: taking the microporous filter membrane off the cup filter, putting the microporous filter membrane into a container, adding ammonia water with the volume concentration of 20-80%, 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 a small amount of water, and collecting filtrate and washing water to obtain a solution in which copper and zinc are dissolved;
D. heating and evaporating a solution obtained after copper and zinc are dissolved to dryness, and acidifying after evaporation to dryness, wherein the acidity of the solution is controlled to be 2-5%; the method specifically comprises the following steps: heating the solution obtained after dissolving copper and zinc to overflow ammonia until the volume is less than or equal to 5mL, slightly cooling, adding nitric acid (1 + 1), controlling the acidity of the solution to be 2-5%, heating and dissolving for 2-20min, cooling, and transferring into a volumetric flask to fix the volume;
E. and (3) measuring copper and zinc in the solution by adopting an atomic absorption spectrum or a plasma spectrum: respectively putting 0, 2.0, 4.0, 8.0 and 10.0mL of copper and zinc standard solutions with the concentration of 10 mu g/mL into a 100mL volumetric flask, adding 2mL of nitric acid into the volumetric flask, fixing the volume with water, measuring the absorbance values of copper and zinc on an atomic absorption spectrometer or a plasma spectrometer by taking water as a reference, and automatically drawing a standard curve by an instrument; on an atomic absorption spectrometer or a plasma spectrometer, the absorbance values of copper and zinc in the solution are measured by taking water as a reference, and the concentrations of the copper and the zinc are checked on a standard curve.
2. The method for measuring trace metals of copper and zinc in nickel-cobalt solution according to claim 1, wherein the method comprises the following steps: and B, when filtering the nickel-cobalt solution in the step B, pouring the nickel-cobalt solution into a cup filter, carrying out suction filtration, enabling all filtrate to pass through the filter membrane, and washing the filter membrane for 2-5 times by using pure water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910214304.0A CN109883971B (en) | 2019-03-20 | 2019-03-20 | Method for measuring trace metal copper and zinc in nickel-cobalt solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910214304.0A CN109883971B (en) | 2019-03-20 | 2019-03-20 | Method for measuring trace metal copper and zinc in nickel-cobalt solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109883971A CN109883971A (en) | 2019-06-14 |
| CN109883971B true CN109883971B (en) | 2021-11-02 |
Family
ID=66933334
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910214304.0A Active CN109883971B (en) | 2019-03-20 | 2019-03-20 | Method for measuring trace metal copper and zinc in nickel-cobalt solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109883971B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113390800B (en) * | 2020-03-13 | 2022-05-20 | 宁德新能源科技有限公司 | Method for detecting content of copper simple substance in lithium battery positive electrode material |
| CN113189088B (en) * | 2021-05-28 | 2022-09-06 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2157819Y (en) * | 1993-03-17 | 1994-03-02 | 安金城 | Filter diaphragm suction filter |
| CN201186179Y (en) * | 2008-01-16 | 2009-01-28 | 王天涯 | Multi-connection stainless steel liquid sample filtration device |
| CN202620830U (en) * | 2012-04-10 | 2012-12-26 | 广东宏盈科技有限公司 | Vacuum filtering device |
| CN102980889A (en) * | 2012-12-07 | 2013-03-20 | 来宾华锡冶炼有限公司 | Method for rapidly detecting zinc content of solution |
| CN103487427A (en) * | 2013-09-27 | 2014-01-01 | 苏州国环环境检测有限公司 | Method for detecting metallic elements in atmospheric exhaust gas particulates |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
-
2019
- 2019-03-20 CN CN201910214304.0A patent/CN109883971B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2157819Y (en) * | 1993-03-17 | 1994-03-02 | 安金城 | Filter diaphragm suction filter |
| CN201186179Y (en) * | 2008-01-16 | 2009-01-28 | 王天涯 | Multi-connection stainless steel liquid sample filtration device |
| CN202620830U (en) * | 2012-04-10 | 2012-12-26 | 广东宏盈科技有限公司 | Vacuum filtering device |
| CN102980889A (en) * | 2012-12-07 | 2013-03-20 | 来宾华锡冶炼有限公司 | Method for rapidly detecting zinc content of solution |
| CN103487427A (en) * | 2013-09-27 | 2014-01-01 | 苏州国环环境检测有限公司 | Method for detecting metallic elements in atmospheric exhaust gas particulates |
| CN103728289A (en) * | 2013-12-16 | 2014-04-16 | 金川集团股份有限公司 | Method for rapidly measuring gold and silver in crude copper |
Non-Patent Citations (4)
| Title |
|---|
| 从弱酸高铁的镍钴溶液中分离杂质;何家金等;《有色金属(冶炼部分)》;19880229;全文 * |
| 流动注射-火焰原子吸收法联用测定钴镍基体中微量杂质元素的应用性研究;李中玺;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20041215(第04期);第34-37页 * |
| 电感耦合等离子体原子发射光谱法测定子午线轮胎用钢帘线镀层中铜含量及镀层厚度;邱月梅等;《理化检验-化学分册》;20151130;第51卷(第11期);"1.1 仪器与试剂"，"1.3.2试样溶液的制备"，"2.3分析谱线的选择"，"2.5标准曲线和检出限" * |
| 能循环滤去镀镍溶液中不溶性机械杂质选择性地吸附除去水溶性有机无机杂质的DP型电镀液过滤机通过鉴定;陈泳林;《电镀与精饰》;19870131;第9卷(第1期);第36页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109883971A (en) | 2019-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109883971B (en) | Method for measuring trace metal copper and zinc in nickel-cobalt solution | |
| Cesur | Determination of manganese, copper, cadmium and lead by FAAS after solid-phase extraction of their phenylpiperazine dithiocarbamate complexes on activated carbon | |
| CN110658143A (en) | Method for measuring contents of trace elements of bismuth, cadmium, chromium, copper, iron, lead, zinc, nickel, cobalt and manganese in high-concentration brine | |
| Tokalıoğlu et al. | Solid phase extraction of Cu (II), Ni (II), Pb (II), Cd (II) and Mn (II) ions with 1-(2-thiazolylazo)-2-naphthol loaded Amberlite XAD-1180 | |
| Zhang et al. | Preconcentration by coprecipitation of arsenic and tin in natural waters with a Ni–pyrrolidine dithiocarbamate complex and their direct determination by solid-sampling atomic-absorption spectrometry | |
| CN109883970A (en) | The method for quantitatively determining of trace silver foreign matter in a kind of cobalt nickel solution | |
| CN107884299B (en) | Method for measuring high zinc slag and organic matters in solution in zinc hydrometallurgy system | |
| Kimura et al. | Preconcentration of traces of silver and bismuth from cobalt and nickel and their nitrates, with activated carbon | |
| Duran et al. | Carrier element-free coprecipitation with 3-phenly-4-o-hydroxybenzylidenamino-4, 5-dihydro-1, 2, 4-triazole-5-one for separation/preconcentration of Cr (III), Fe (III), Pb (II) and Zn (II) from aqueous solutions | |
| Hassanien | Silica glass modified with flavonoid derivatives for preconcentration of some toxic metal ions in water samples and their determination with ICP-MS | |
| Akcin et al. | Determination of zinc, nickel and cadmium in natural water samples by flame atomic absorption spectrometry after preconcentration with ion exchange and flotation techniques | |
| Gustin et al. | Spectrophotometric Determination of Palladium with 8-Aminoquinoline. | |
| CN111122548A (en) | Method for detecting trace metal copper and zinc in lithium carbonate | |
| CN112179894A (en) | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery | |
| CN104914262B (en) | The chromic automatic analysis method of trace in water sample | |
| Hibbard | Micromethods for determination of zinc | |
| van der Sloot et al. | The determination of vanadium in sea and surface waters | |
| Frigge et al. | Systematic investigation of multi-element preconcentration from copper alloys by carbamate precipitation before atomic absorption spectrometric analysis | |
| CN114014422B (en) | Metal ion separation and enrichment system and method for separating and enriching cobalt (II) | |
| Burns et al. | Spectrophotometric determination of bismuth after extraction of 1-naphthylmethyltriphenylphosphonium tetraiodobismuthate (III) | |
| van Elteren et al. | Determination of ultratrace dissolved arsenite in water–selective coprecipitation in the field combined with HGAFS and ICP–MS measurement in the laboratory | |
| CN109540878B (en) | Kit for detecting barium ions and detection method thereof | |
| Taruki et al. | Determination of tin by resin-suspension electrothermal atomic absorption spectrometry after enrichment as the complex with ammonium pyrrolidinedithiocarbamate | |
| CN108088804B (en) | A kind of measuring method of trace cadmium in water samples | |
| El-Menshawy et al. | Zincon polymer as a new modifier for selective separation and determination of copper and zinc from synthetic, water and drug samples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |