CN109883971A - Trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution - Google Patents
Trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution Download PDFInfo
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Abstract
The invention discloses trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution, this method is filtered nickel and cobalt solution using miillpore filter, so that the metal simple-substance in nickel and cobalt solution stays on filter membrane, then selective dissolution is carried out to metallic copper, zinc or its alloy on miillpore filter using ammonium hydroxide, to make metallic copper, zinc on filter membrane enter solution, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry after treatment, obtain the content of GOLD FROM PLATING SOLUTION category copper, zinc.Present invention process is simple, can effectively detect trace meter copper, zinc in solution, and testing result is accurate and reliable, and treated, and solution can directly return to production line, not will cause the waste of material.Trace meter copper, Direct spectrophotometry the mixed solution with other metals of the present invention suitable for nickel sulfate, cobalt chloride, cobalt nitrate, cobaltous sulfate and nickel cobalt mixed solution or based on nickel cobalt.
Description
Technical field
The invention belongs to chemical analysis technology fields, and in particular to trace meter in a kind of battery material nickel and cobalt solution
Copper, Direct spectrophotometry method.
Background technique
The solution of nickel can be used to the salt type materials such as extracting sulfuric acid nickel or nickel hydroxide, it is also possible to manufacture nickel cobalt manganese, nickel cobalt
The ternary oxide of the types such as aluminium, cobalt liquor can be used to make the ternary oxide of cobaltosic oxide or cobalt, these materials are available
In manufacture nickel-metal hydride battery or for manufacturing lithium ion battery, nickel-metal hydride battery or lithium ion battery to metallic foreign bodies such as silver, copper, zinc
There is very high requirement, will lead to safety accident beyond content range, therefore, the company for producing battery material can be to entirely producing
The monitoring of Cheng Jinhang foreign matter, including nickel solution therein, cobalt liquor.The influence of battery producer metallic foreign body is not only depending on foreign matter
Content additionally depends on the size of foreign matter, and the in general foreign matter of size 0.8um or more is harmful.
Metallic copper in nickel, cobalt liquor, zinc source may be environmental factor, it is also possible to the mill of production process relevant device
Damage introduces, and content is humble, uses conventional sour processing method that cannot effectively detect therein with micro gold existing for metallic state
Belong to copper zinc.
Summary of the invention
The purpose of the present invention is to solve the technical problems existing in the prior art, provide a kind of simple process, can have
Effect detects trace meter copper, Direct spectrophotometry method in trace meter copper zinc and the accurate nickel and cobalt solution of testing result.
In order to achieve the above object, the invention adopts the following technical scheme: trace meter copper in a kind of nickel and cobalt solution, zinc
Measuring method, method includes the following steps:
A, miillpore filter is fixed on cup type filter, connects filter and vacuum pump, opened vacuum pump switch, washed with pure water
Wash filter membrane；
B, nickel and cobalt solution is filtered using miillpore filter, so that the metal simple-substance in nickel and cobalt solution stays on filter membrane；
C, miillpore filter is used into AMMONIA TREATMENT, dissolves the metallic copper zinc on miillpore filter；
D, the solution heating obtained after the dissolution of copper zinc is evaporated, is acidified after being evaporated, control solution acidity is 2-5%；
E, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry.
Further, nickel and cobalt solution is poured into cup type filter when being filtered in the step B to nickel and cobalt solution, is taken out
Filter, makes filtrate all pass through filter membrane, with pure water filter membrane 2-5 times.
Further, miillpore filter is used to the specific steps of AMMONIA TREATMENT are as follows: by miillpore filter from cup in the step C
It removes and is put into container on formula filter, the ammonium hydroxide that volumetric concentration is 20-80%, low-temperature heat 5-20min, after cooling is added
Filtering with microporous membrane is used on cup type filter, filter membrane is washed with a small amount 3-6 times, collects filtrate and wash water obtains the dissolution of copper zinc
Solution afterwards.
Further, the specific steps of the step D are as follows: the solution obtained after the dissolution of copper zinc is heated, overflows ammonia, directly
It is slightly cold to volume≤5mL, it is added nitric acid (1+1), control solution acidity is 2-5%, dissolves by heating 2-20min, moves into after cooling
Constant volume in volumetric flask.
Further, the specific steps that the step E is measured are as follows: take 0,2.0,4.0,8.0,10.0mL concentration respectively
It is the copper of 10ug/mL, Zinc standard solution in 100mL volumetric flask, 2mL nitric acid is added in volumetric flask, with water constant volume, in atom
On absorption spectrometer or plasma spectrometer, using water as reference, the absorbance value of measurement copper, zinc, instrument draws standard automatically
Curve；On Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, the absorbance value of copper, zinc in solution is measured,
Copper, zinc concentration are checked in standard curve.
The present invention has the advantages that the survey of trace meter copper, zinc in nickel and cobalt solution of the present invention compared with the prior art
Determine method to be filtered nickel and cobalt solution using miillpore filter, so that the metal simple-substance in nickel and cobalt solution stays on filter membrane, then
Selective dissolution is carried out to metallic copper, zinc or its alloy on miillpore filter using ammonium hydroxide, to make the metallic copper on filter membrane, zinc
Into solution, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry after treatment, obtained
The content of GOLD FROM PLATING SOLUTION category copper, zinc.Present invention process is simple, can effectively detect trace meter copper, zinc in solution, detection knot
Fruit is accurate and reliable, and treated, and solution can directly return to production line, not will cause the waste of material.The present invention is suitable for sulfuric acid
It is micro- in nickel, cobalt chloride, cobalt nitrate, cobaltous sulfate and nickel cobalt mixed solution or the mixed solution with other metals based on nickel cobalt
Measure metallic copper, Direct spectrophotometry.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1
A, the water system miillpore filter that diameter is 50mm, aperture is 0.8um is fixed on cup type filter, connection filter and true
Sky pump, opens vacuum pump switch, with 50mL pure water filter membrane.
B, 500mL cobalt nitrate solution is poured into cup type filter, filters, so that filtrate is all passed through filter membrane, washed with pure water
It washs filter membrane 2 times, water 10mL is used every time, so that the metal simple-substance in cobalt nitrate solution stays on filter membrane.
C, by miillpore filter from removing and being put into 200mL beaker on cup type filter, the ammonia that volumetric concentration is 20% is added
Water, low-temperature heat 5min dissolve the metallic copper zinc on miillpore filter, are filtered on cup type filter with 0.45um micropore after cooling
Film filtering, is washed with a small amount filter membrane 3 times, collects filtrate and wash water obtains copper zinc dissolved solution, be transferred to 200mL beaker
In.
D, the solution obtained after copper zinc dissolution in beaker is heated, overflows the ammonia in beaker, until volume≤5mL, slightly
It is cold, it is added nitric acid (1+1), control solution acidity is 2%, dissolves by heating 10min, moves into constant volume in volumetric flask after cooling.
E, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry: take 0 respectively, 2.0,
4.0,8.0,10.0mL concentration is the copper of 10ug/mL, Zinc standard solution in 100mL volumetric flask, and 2mL nitre is added in volumetric flask
Acid, with water constant volume, on Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, the absorbance of measurement copper, zinc
Value, instrument draw standard curve automatically；On Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, measure molten
The absorbance value of copper, zinc in liquid checks in copper, zinc concentration in standard curve.
Embodiment 2
A, the water system miillpore filter that diameter is 47mm, aperture is 1.0um is fixed on cup type filter, connection filter and true
Sky pump, opens vacuum pump switch, with 50mL pure water filter membrane.
B, 1000mL nickel sulfate solution is poured into cup type filter, filters, so that filtrate is all passed through filter membrane, washed with pure water
It washs filter membrane 5 times, water 10mL is used every time, so that the metal simple-substance in nickel sulfate solution stays on filter membrane.
C, by miillpore filter from removing and being put into 200mL beaker on cup type filter, the ammonia that volumetric concentration is 80% is added
Water, low-temperature heat 20min dissolve the metallic copper zinc on miillpore filter, and 0.30um micropore is used on cup type filter after cooling
Membrane filtration is washed with a small amount filter membrane 6 times, collects filtrate and wash water obtains copper zinc dissolved solution, be transferred to 200mL beaker
In.
D, the solution obtained after copper zinc dissolution in beaker is heated, overflows the ammonia in beaker, until volume≤5mL, slightly
It is cold, it is added nitric acid (1+1), control solution acidity is 5%, dissolves by heating 20min, moves into constant volume in volumetric flask after cooling.
E, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry: take 0 respectively, 2.0,
4.0,8.0,10.0mL concentration is the copper of 10ug/mL, Zinc standard solution in 100mL volumetric flask, and 2mL nitre is added in volumetric flask
Acid, with water constant volume, on Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, the absorbance of measurement copper, zinc
Value, instrument draw standard curve automatically；On Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, measure molten
The absorbance value of copper, zinc in liquid checks in copper, zinc concentration in standard curve.
Embodiment 3
A, the water system miillpore filter that diameter is 50mm, aperture is 1.0um is fixed on cup type filter, connection filter and true
Sky pump, opens vacuum pump switch, with 50mL pure water filter membrane.
B, the mixed solution of 2000mL nickel sulfate and cobaltous sulfate is poured into cup type filter, is filtered, keep filtrate all logical
Filter membrane uses water 10mL, so that the metal list in the mixed solution of nickel sulfate and cobaltous sulfate with pure water filter membrane 3 times every time
Matter stays on filter membrane.
C, by miillpore filter from removing and being put into 200mL beaker on cup type filter, the ammonia that volumetric concentration is 50% is added
Water, low-temperature heat 10min dissolve the metallic copper zinc on miillpore filter, and 0.30um micropore is used on cup type filter after cooling
Membrane filtration is washed with a small amount filter membrane 5 times, collects filtrate and wash water obtains copper zinc dissolved solution, be transferred to 200mL beaker
In.
D, the solution obtained after copper zinc dissolution in beaker is heated, overflows the ammonia in beaker, until volume≤5mL, slightly
It is cold, it is added nitric acid (1+1), control solution acidity is 3%, dissolves by heating 2min, moves into constant volume in volumetric flask after cooling.
E, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry: take 0 respectively, 2.0,
4.0,8.0,10.0mL concentration is the copper of 10ug/mL, Zinc standard solution in 100mL volumetric flask, and 2mL nitre is added in volumetric flask
Acid, with water constant volume, on Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, the absorbance of measurement copper, zinc
Value, instrument draw standard curve automatically；On Atomic Absorption Spectrometer or plasma spectrometer, using water as reference, measure molten
The absorbance value of copper, zinc in liquid checks in copper, zinc concentration in standard curve.
The determination condition of atomic absorption spectrography (AAS) and plasma spectroscopy is as shown in Table 1 and Table 2 in above-described embodiment:
1 aas determination condition of table
2 plasma spectroscopy measuring method of table
Claims (5)
1. trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution, it is characterised in that method includes the following steps:
A, miillpore filter is fixed on cup type filter, connects filter and vacuum pump, opened vacuum pump switch, washed with pure water
Wash filter membrane；
B, nickel and cobalt solution is filtered using miillpore filter, so that the metal simple-substance in nickel and cobalt solution stays on filter membrane；
C, miillpore filter is used into AMMONIA TREATMENT, dissolves the metallic copper zinc on miillpore filter；
D, the solution heating obtained after the dissolution of copper zinc is evaporated, is acidified after being evaporated, control solution acidity is 2-5%；
E, copper, the zinc in solution are measured using atomic absorption spectrum or plasma spectrometry.
2. trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution according to claim 1, it is characterised in that: institute
It states and pours into nickel and cobalt solution in cup type filter when being filtered in step B to nickel and cobalt solution, filter, filtrate is made all to pass through filter
Film, with pure water filter membrane 2-5 times.
3. trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution according to claim 1, it is characterised in that: institute
State the specific steps that miillpore filter is used to AMMONIA TREATMENT in step C are as follows: miillpore filter is removed and put from cup type filter
Enter in container, the ammonium hydroxide that volumetric concentration is 20-80%, low-temperature heat 5-20min, with micro- on cup type filter after cooling is added
Hole membrane filtration, is washed with a small amount filter membrane 3-6 times, collects filtrate and wash water obtains copper zinc dissolved solution.
4. trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution according to claim 1, it is characterised in that: institute
State the specific steps of step D are as follows: the solution obtained after the dissolution of copper zinc is heated, ammonia is overflowed, until volume≤5mL, slightly cold, adds
Enter nitric acid (1+1), control solution acidity is 2-5%, dissolves by heating 2-20min, moves into constant volume in volumetric flask after cooling.
5. trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution according to claim 1, it is characterised in that: institute
State the specific steps that step E is measured are as follows: take 0,2.0,4.0,8.0, copper, the zinc mark that 10.0mL concentration is 10ug/mL respectively
In 100mL volumetric flask 2mL nitric acid is added, with water constant volume, in Atomic Absorption Spectrometer or plasma in quasi- solution in volumetric flask
On body spectrometer, using water as reference, the absorbance value of measurement copper, zinc, instrument draws standard curve automatically；In atomic absorption spectrum
On instrument or plasma spectrometer, using water as reference, the absorbance value of copper, zinc in solution is measured, checks in copper, zinc in standard curve
Concentration.
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| 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 |
| CN113189088A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
| CN113390800A (en) * | 2020-03-13 | 2021-09-14 | 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 |
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