CN114397400B - Method for measuring nickel and cobalt content in nickel and cobalt mixed salt - Google Patents
Method for measuring nickel and cobalt content in nickel and cobalt mixed salt Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 34
- 239000010941 cobalt Substances 0.000 title claims abstract description 34
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 32
- 150000003839 salts Chemical class 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 15
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims abstract description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012086 standard solution Substances 0.000 claims abstract description 28
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 14
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims abstract description 12
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003926 complexometric titration Methods 0.000 claims abstract description 6
- 238000004448 titration Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 4
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 13
- 239000011521 glass Substances 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- JJRVRELEASDUMY-JXMROGBWSA-N (5e)-5-[[4-(dimethylamino)phenyl]methylidene]-2-sulfanylidene-1,3-thiazolidin-4-one Chemical compound C1=CC(N(C)C)=CC=C1\C=C\1C(=O)NC(=S)S/1 JJRVRELEASDUMY-JXMROGBWSA-N 0.000 description 3
- -1 potassium ferricyanide Chemical compound 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 description 2
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 description 2
- 235000010703 Modiola caroliniana Nutrition 0.000 description 2
- 244000038561 Modiola caroliniana Species 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
- G01N21/83—Turbidimetric titration
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
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Abstract
The invention discloses a method for measuring the content of nickel and cobalt in nickel-cobalt mixed salt, which comprises the following steps: s1, taking a part of nickel-cobalt mixed salt sample, and measuring the content of c (Ni) +c (Co) by using EDTA complexometric titration; s2, another part of nickel-cobalt mixed salt sample is taken, quantitative and excessive potassium cyanide standard solution is added, and silver nitrate back titration is used for measuring excessive cyanide ions, so that the content of 4c (Ni) +5c (Co) is calculated; s3, calculating the nickel content and the cobalt content in the nickel-cobalt mixed salt. The advantages are that: the detection method disclosed by the invention does not need large-scale equipment such as ICPOES and the like, and can be used for rapidly and accurately analyzing the content of nickel and cobalt in the nickel-cobalt mixed salt by only using a glass instrument commonly used in a laboratory, so that the detection cost can be obviously saved, and the detection efficiency and the detection precision can be improved.
Description
Technical Field
The invention relates to a nonferrous metal analysis and detection technology, in particular to a detection method for nickel and cobalt content in nickel and cobalt mixed salt.
Background
Nickel and cobalt are two important metals in nonferrous metal industry, and in recent years, due to the rapid development of new energy materials, the value of the new energy materials is increasingly valued, and the accurate, precise and rapid measurement of the nickel and cobalt content in the nickel and cobalt mixed salt has great significance for nickel and cobalt metal processing and using manufacturers.
In the conventional constant nickel-cobalt detection method, nickel is mainly determined by a dimethylglyoxime weight method, cobalt is mainly determined by a potassium ferricyanide potentiometric titration method, and the dimethylglyoxime weight method is complex in operation, long in test process and unfavorable for guiding production; however, the potassium ferricyanide potentiometric titration method can only detect cobalt, and for high-content nickel-cobalt mixed salts in which nickel and cobalt exist in large quantities simultaneously, if the content of nickel and cobalt in a solution is to be rapidly determined, a conventional EDTA complexometric titration method is generally used for determining the content of nickel and cobalt, then an ICP-OES method is used for determining the ratio of nickel and cobalt, and the content of nickel and cobalt is calculated by combining the content of nickel and cobalt.
Disclosure of Invention
The invention provides a method for measuring the content of nickel and cobalt in nickel and cobalt mixed salt, which is used for simplifying the detection of the content of nickel and cobalt in the nickel and cobalt mixed salt.
The technical scheme adopted by the invention is as follows: the method for measuring the nickel-cobalt content in the nickel-cobalt mixed salt comprises the following steps:
s1, taking a part of nickel-cobalt mixed salt sample, and measuring the content of c (Ni) +c (Co) by using EDTA complexometric titration;
s2, another part of nickel-cobalt mixed salt sample is taken, quantitative and excessive potassium cyanide standard solution is added, and silver nitrate back titration is used for measuring excessive cyanide ions, so that the content of 4c (Ni) +5c (Co) is calculated;
s3, obtaining the nickel content and cobalt content in the nickel-cobalt mixed salt through the formula (1) and the formula (2):
c (Ni) =5× [ c (Ni) +c (Co) content ] - [4c (Ni) +5c (Co) content ] (1)
c (Co) = [4c (Ni) +5c (Co) content ] -4× [ c (Ni) +c (Co) content ] (2)
The invention skillfully utilizes the characteristics that coordination numbers of nickel (II) ions, cobalt (II) ions and EDTA are 1, and coordination numbers of the cobalt (II) ions and cyanide ions are 4 and 5 respectively to determine the nickel and cobalt content in the nickel and cobalt mixed salt, thereby simplifying the existing detection method.
Wherein, the step S1 can be implemented according to the following specific scheme: taking a part of nickel-cobalt mixed salt sample, preparing a solution, and then measuring the content of c (Ni) +c (Co) in an ammonia-ammonium chloride buffer solution with the pH value of 9-11 by using ammonium violurate as an indicator and EDTA complexometric titration.
Wherein, the step S2 can be implemented according to the following specific scheme: taking another part of nickel-cobalt mixed salt sample, preparing a solution, regulating the nickel-cobalt mixed salt solution to be slightly alkaline, namely, pH (potential of hydrogen) approximately equal to 11.5-12 and ammonia content 1-2 g/L, adding a reducing agent ascorbic acid to inhibit oxidation of cobalt ions in an ammoniacal high-cyanide environment, then adding a quantitative and excessive potassium cyanide standard solution, and complexing cyanide ions with nickel ions and cobalt ions; excess cyanide ions were then measured by back titration with silver nitrate, and the 4c (Ni) +5c (Co) content was calculated.
The beneficial effects of the invention are as follows: the detection method disclosed by the invention does not need large-scale equipment such as ICPOES and the like, and can be used for rapidly and accurately analyzing the content of nickel and cobalt in the nickel-cobalt mixed salt by only using a glass instrument commonly used in a laboratory, so that the detection cost can be obviously saved, and the detection efficiency and the detection precision can be improved.
Detailed Description
The invention is further illustrated below with reference to examples.
Examples:
firstly, preparing a standard solution and calibrating:
(1) preparing a part of nickel-cobalt mixed salt solution containing 1.8000g/L and 1.2000g/L of cobalt by using a standard substance with a certificate as a working standard reagent of the nickel-cobalt mixed salt;
(2) preparing 0.02mol/L EDTA standard solution, taking 10mL of nickel-cobalt mixed salt working standard reagent into a 250mL conical flask, adding 10mL of ammonia-ammonium chloride buffer solution with pH value of 10, adding 0.2g of 2% ammonium purple urea indicator, and taking the final point as the end point when the calibrated EDTA standard solution is titrated to mauve. EDTA standard solution concentration= (nickel concentration 1.8000g/L ++nickel atomic weight 58.693 g/mol+cobalt concentration 1.2000g/L ++cobalt atomic weight 58.933 g/mol). Times.nickel cobalt mixed salt working standard reagent split volume 10mL ++EDTA standard solution consumption volume 25.25mL = 0.02021mol/L;
(3) preparing 0.05mol/L silver nitrate standard solution, weighing 1.0005g of sodium chloride working standard reagent which is burned to constant weight in a muffle furnace at 550 ℃, after dissolving, fixing the volume to 250mL, shaking uniformly, taking 25.00mL in a 250mL conical flask, adding 4 drops of 2g/L p-dimethylaminobenzylidene rhodamine indicator, taking the end point when the silver nitrate solution to be calibrated is titrated to change from yellow to orange red, wherein the concentration of the silver nitrate standard solution = the mass of the sodium chloride working standard reagent is 1.0005 g/100 mL of the fixed volume x 10 mL/mol of the split volume x the molecular weight of sodium chloride is 58.443 g/mol/silver nitrate standard solution consumption volume 34.19mL x 1000mL/L = 0.05007mol/L;
(4) preparing 0.1mol/L potassium cyanide standard solution, accurately dividing 25mL of the potassium cyanide standard solution to be calibrated into a 250mL conical flask, adding 4 drops of 2g/L p-dimethylaminobenzylidene rhodamine indicator, and taking the end point when the calibrated 0.05mol/L silver nitrate standard solution is titrated to yellow to orange red, wherein the consumption volume of the potassium cyanide standard solution=2×silver nitrate standard solution 0.05007mol/L×silver nitrate standard solution is 25.48mL, and the dividing volume of the potassium cyanide standard solution is 25 mL= 0.1021mol/L.
Secondly, determining the content of c (Ni) +c (Co) in the sample to be detected: accurately diluting a sample and accurately separating a proper amount of solution to ensure that the nickel cobalt content is not more than 50mg, adding 10mL of ammonia-ammonium chloride buffer solution with pH=10 and 0.2g of 2% ammonium violate indicator, and taking titration of EDTA standard solution to mauve as an end point, wherein the content of c (Ni) +c (Co) =the concentration of EDTA standard solution 0.02021mol/L×the consumption volume of EDTA standard solution is 25.05 mL/nickel cobalt mixed salt diluted solution, and the separation volume of 10mL×the dilution multiple of nickel cobalt mixed salt is 50= 2.531mol/L.
Third, the content of 4c (Ni) +5c (Co) is determined: accurately diluting a sample by 50 times, accurately separating 10mL of the sample from a 250mL conical flask, adding water to 50mL of the sample, adding 1mL of 10% ammonia water and 0.2g of ascorbic acid, adjusting the pH to be approximately equal to 11.5 by 1mol/L of dilute alkali, adding 50mL of standardized potassium cyanide standard solution on the same day, adding 4 drops of 2g/L of p-dimethylaminobenzylidene rhodamine indicator, titrating the 0.05mol/L of silver nitrate standard solution to change yellow into orange red to obtain the end point, and separating the 10mL of nickel cobalt mixed salt diluted solution by 50 = 10.990mol/L according to the concentration of 4c (Ni) +5c (Co) = (the concentration of the potassium cyanide standard solution is 0.1021mol/L, the concentration of the potassium cyanide standard solution is 0.05007mol/L, the consumption volume of the silver nitrate standard solution is 29.03 mL).
Fourth, resolving nickel content and cobalt content:
C (Ni) (g/L) = (5× [ c (Ni) +c (Co) content](mol/L)－[4c(Ni)+5c(Co)](mol/L))×58.69g/mol＝97.72g/L；
C (Co) (mol/L) = [4c (Ni) +5c (Co) content](mol/L) -4 x [ c (Ni) +c (Co) content](mol/L)×58.93g/mol＝51.03g/L。
Claims (1)
1. The method for measuring the nickel-cobalt content in the nickel-cobalt mixed salt comprises the following steps:
s1, taking a part of nickel-cobalt mixed salt sample, and measuring the content of c (Ni) +c (Co) by using EDTA complexometric titration; the method for measuring the c (Ni) +c (Co) content in the step S1 specifically comprises the following steps: taking a part of nickel-cobalt mixed salt sample, preparing a solution, and then measuring the content of c (Ni) +c (Co) in an ammonia-ammonium chloride buffer solution with the pH value of 9-11 by using ammonium violurate as an indicator and EDTA complexometric titration;
s2, another part of nickel-cobalt mixed salt sample is taken, quantitative and excessive potassium cyanide standard solution is added, and silver nitrate back titration is used for measuring excessive cyanide ions, so that the content of 4c (Ni) +5c (Co) is calculated; the method for measuring the content of 4c (Ni) +5c (Co) in the step S2 specifically comprises the following steps: another part of nickel-cobalt mixed salt sample is taken, after the solution is prepared, the pH value of the nickel-cobalt mixed salt solution is regulated to 11.5-12, the ammonia content is 1-2 g/L, a reducing agent ascorbic acid is added to inhibit the oxidation of cobalt ions in an ammoniacal high-cyanide environment, then a quantitative and excessive potassium cyanide standard solution is added, and cyanide ions are complexed with nickel ions and cobalt ions; then, the excess cyanide ions are measured by back titration with silver nitrate, so that the content of 4c (Ni) +5c (Co) is calculated;
s3, obtaining the nickel content and cobalt content in the nickel-cobalt mixed salt through the formula (1) and the formula (2):
c (Ni) =5× [ c (Ni) +c (Co) content ] - [4c (Ni) +5c (Co) content ] (1);
c (Co) = [4c (Ni) +5c (Co) content ] -4× [ c (Ni) +c (Co) content ] (2).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636616A (en) * | 2012-03-21 | 2012-08-15 | 云南昆钢煤焦化有限公司 | Method for testing content of hydrogen cyanide in gas |
| CN106290334A (en) * | 2016-08-05 | 2017-01-04 | 江苏理工学院 | Cobalt and the chemistry in detecting of Fe content in cobalt manganese raw material |
| CN108226143A (en) * | 2016-12-13 | 2018-06-29 | 天津国安盟固利新材料科技股份有限公司 | A kind of method for detecting nickel cobalt manganese content in ternary material or ternary precursor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636616A (en) * | 2012-03-21 | 2012-08-15 | 云南昆钢煤焦化有限公司 | Method for testing content of hydrogen cyanide in gas |
| CN106290334A (en) * | 2016-08-05 | 2017-01-04 | 江苏理工学院 | Cobalt and the chemistry in detecting of Fe content in cobalt manganese raw material |
| CN108226143A (en) * | 2016-12-13 | 2018-06-29 | 天津国安盟固利新材料科技股份有限公司 | A kind of method for detecting nickel cobalt manganese content in ternary material or ternary precursor |
Non-Patent Citations (5)
| Title |
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| 918碱性锌镍镀液中锌、镍离子的测定;吴新花;西北地质;第19卷(第3期);第53-55页 * |
| CONTRIBUTIONS TO THE BASIC PROBLEMS OF COMPLEXOMETRY-XXI* DETERMINATION OF NICKEL IN THE PRESENCE OF COBALT;RUDOLF PRIBIL等;Talanta;第13卷;第515-518页 * |
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