CN116008378A - Electrolyte for detecting cobalt element by anodic stripping voltammetry and cobalt element detection method - Google Patents
Electrolyte for detecting cobalt element by anodic stripping voltammetry and cobalt element detection method Download PDFInfo
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 119
- 239000010941 cobalt Substances 0.000 title claims abstract description 119
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000003792 electrolyte Substances 0.000 title claims abstract description 70
- 238000001514 detection method Methods 0.000 title claims abstract description 37
- 238000003968 anodic stripping voltammetry Methods 0.000 title claims abstract description 20
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 30
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 7
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- 238000005259 measurement Methods 0.000 claims description 26
- -1 amine compounds Chemical class 0.000 claims description 25
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- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 19
- 238000004090 dissolution Methods 0.000 claims description 18
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- 229910001385 heavy metal Inorganic materials 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 11
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- 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
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 6
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
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- 239000004471 Glycine Substances 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
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- 235000006408 oxalic acid Nutrition 0.000 claims description 2
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- 238000012544 monitoring process Methods 0.000 abstract description 6
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- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 238000003950 stripping voltammetry Methods 0.000 description 4
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 3
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- 229910001429 cobalt ion Inorganic materials 0.000 description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
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- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
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- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The application relates to the technical field of water quality monitoring, and particularly discloses electrolyte for detecting cobalt element by an anodic stripping voltammetry and a cobalt element detection method. An electrolyte for detecting cobalt element by an anodic stripping voltammetry method comprises the following substances: 0.1-1 mol/L ammonium chloride, 20-80 g/L additive and 7-49 mL/L concentrated ammonia water. The detection method comprises the following steps: and detecting and calculating the concentration of cobalt element in the sample by using a three-electrode system. The electrolyte can be used for detecting cobalt element and has the advantages of strong anti-interference capability, excellent reproducibility, low cost and simplicity in operation.
Description
Technical Field
The application relates to the technical field of water quality monitoring, in particular to a method for continuously, accurately, simply, conveniently and rapidly detecting cobalt element in water by using an anodic stripping voltammetry; in particular to an electrolyte for detecting cobalt element by an anodic stripping voltammetry and a cobalt element detection method.
Background
Cobalt (Co) is one of the microelements necessary for human body, and can stimulate hematopoiesis, affect fat metabolism, participate in the synthesis of protein amino-coenzyme, lipoprotein and the like, and are closely related to the health of human beings. Cobalt deficiency in the human body can affect the formation of red blood cells, and giant cell anemia occurs. Of course, the uptake of cobalt is not as good as the more. Excessive ingestion of cobalt and cobalt compounds via the respiratory tract, esophagus, skin and blood may cause allergic asthma, gastrointestinal dysfunction, irritant dermatitis and erythrocyte excess. Cobalt and cobalt oxides are classified as class 2B carcinogens in the list of carcinogens published by the world health organization.
Cobalt is very low in concentration in natural water, and waste water of enterprises such as nonferrous metal smelting, cobalt-containing material processing and the like often contains high-concentration cobalt, and if the cobalt is discharged into the environment without proper treatment, the life and health of human beings can be influenced or even endangered. Currently, cobalt determination is involved in pollution condition investigation of surface water source, groundwater and soil monitoring of drinking water.
Currently, the dominant methods for cobalt determination are atomic absorption, inductively coupled plasma mass spectrometry and spectrophotometry. The first two are mature, but instrument consumables are expensive; the latter is simple to operate and rapid to detect, but has high detection limit and poor selectivity. In addition, the stripping voltammetry has the characteristics of low cost, high sensitivity and rapid detection. The principle is that the trace amount of the measured object in the electrolyte is concentrated on the electrode by electrolysis, and then the electrode is scanned by reverse potential, so that the component is dissolved out and the voltammogram is recorded. Qualitative in terms of the position of the elution potential and quantitative in terms of the magnitude of the elution current.
The report of the stripping voltammetry for measuring cobalt element comprises (1) the combination of a mercury suspension electrode and an ammonium chloride-dimethylglyoxime system electrolyte; (2) the glassy carbon electrode is matched with sodium hydroxide-5-Br-PADAP system electrolyte; (3) the carbon paste electrode is matched with an ammonium chloride-phenanthroline system electrolyte; (4) the Nafion modified glassy carbon electrode is matched with sodium nitrate electrolyte. The methods essentially belong to cathode dissolution methods, the electrode surface involves adsorption or catalysis processes, most of the methods need electrode modification, the reproducibility of the results is poor, the requirements on mass production of the electrodes are high, and the methods are not suitable for wide application in terms of cost, operation and the like. Therefore, for cobalt determination, a test method with strong anti-interference capability, good reproducibility, low cost and simple operation is developed, and the test method has a relatively high application prospect.
Disclosure of Invention
In order to obtain the cobalt element testing method with strong anti-interference capability, good reproducibility, low cost and simple operation, the application provides the electrolyte for detecting the cobalt element by the anodic stripping voltammetry and the cobalt element detection method.
In a first aspect, the present application provides an electrolyte for detecting cobalt element by anodic stripping voltammetry, which adopts the following technical scheme:
an electrolyte for detecting cobalt element by an anodic stripping voltammetry method comprises the following substances: 0.1-1 mol/L ammonium chloride, 20-80 g/L additive and 7-49 mL/L concentrated ammonia (the mass fraction of the concentrated ammonia is 25-28% per 30mL is diluted into 1000mL of water).
Through adopting above-mentioned technical scheme, detect the content of cobalt element through positive pole stripping voltammetry in this application technical scheme, its principle is through applying invariable voltage to the electrode that soaks in specific electrolyte, when the voltage of selecting reaches the electrolysis reduction potential of the cobalt ion (or the cooperation ion) that awaits measuring, cobalt ion (or cooperation ion) can migrate to the electrode surface, takes place the reduction reaction, and this is the enrichment stage. After the enrichment is completed and the static is carried out for a short time, the voltage on the electrode is reversely increased at a certain rate, cobalt enriched on the surface of the electrode can undergo oxidation reaction and dissolve out to generate oxidation current, and quantitative measurement is carried out according to the peak current of the dissolution peak in a current-voltage curve. The analysis method is sensitive, and the detection limit can reach 10 -12 mol/L, the detection accuracy of cobalt element is better.
In the present application, ammonium chloride and strong ammonia water are preferably used as electrolyte to form NH 3 -NH 4 The Cl buffer system enables cobalt element to show an anode dissolution peak on the voltammetric graph under the action of an external electric field and under specific electrochemical parameters, so that the content of the cobalt element is conveniently calculated. Ammonium chloride has a certain influence on the dissolution peak of cobalt element and can be used as supporting electricityThe electrolyte increases the potential difference of each ion dissolution peak, improves the sharpness of the peak, and improves the sensitivity for monitoring cobalt element.
Preferably, the additive is selected from any one or more of fluoride, amine compounds or organic acids.
Through adopting above-mentioned technical scheme, adopt in this application technical scheme to increase the additive in electrolyte, fluoride, amine compound and organic acid all can be as the masking agent, through complexing reaction, redox reaction or precipitation reaction, get rid of iron ion, nickel ion and manganese ion etc. in the sample, eliminate the influence of other metal ions in the sample to cobalt element detection, improved the precision that cobalt element detected. And fluoride, cyanide and organic acid can be mutually matched, so that the combination effect of the additive and iron ions, nickel ions, manganese ions and the like in the sample is improved, interference peaks are eliminated, and the accuracy of detection results is improved.
Preferably, the organic acid is selected from any one of ascorbic acid, citric acid, oxalic acid or glycine.
Preferably, the fluoride is selected from any one of sodium fluoride, potassium fluoride, ammonium fluoride and ammonium bifluoride.
Preferably, the amine compound is selected from triethanolamine or hydroxylamine hydrochloride.
Through adopting above-mentioned technical scheme, the fluoride of preferred adoption in this application technical scheme is as electrolyte additive, and fluoride ion can carry out complex reaction with other metal ions in the sample, such as iron ion, nickel ion and manganese ion, can stably reduce other metal ions to cobalt element testing result's influence, eliminates the interference peak, improves cobalt element's detection accuracy.
Preferably, the fluoride is ammonium fluoride.
By adopting the technical scheme, the ammonium fluoride is preferably selected as the additive in the technical scheme, and not only contains fluoride ions, but also contains ammonium ions, so that other metal ions in a sample can be effectively combined, and interference peaks are eliminated. Meanwhile, in order to improve the sensitivity of cobalt element determination, the concentration of the electrolyte is selected to be relatively high. The ammonia water is more volatile, so that the concentration of ammonium ions in the electrolyte is reduced, namely the problem that the conductive effect of the electrolyte is poor, and the ammonium ions in the electrolyte can be supplemented through the addition of ammonium fluoride, so that the concentration stability of the ammonium ions in the electrolyte is maintained, and the accuracy, stability and sensitivity of cobalt element detection are kept at higher levels.
Preferably, the material is prepared from the following substances in percentage by weight: 0.5mol/L ammonium chloride, 30mL/L concentrated ammonia (25% -28% of the mass fraction of the concentrated ammonia is diluted into 1000mL of water per 30 mL) and 45g/L ammonium fluoride.
Through adopting above-mentioned technical scheme, optimized the constitution and the additive amount of electrolyte in this application technical scheme, suitable ammonium fluoride additive amount effectively masks metal ions such as iron ion, nickel ion and manganese ion in the sample, and less to the influence of cobalt ion, cobalt element can be stabilized and remove under the effect of electric field and precipitate at the positive pole to the linearity of the volt-ampere curve that obtains is preferred, has further improved the accuracy that cobalt element detected.
In a second aspect, the present application provides a method for detecting cobalt element, which adopts the following technical scheme:
a cobalt element detection method, which uses an anode stripping voltammetry to detect cobalt element electrolyte, comprises the following steps:
a) Inserting a counter electrode into the counter electrode socket;
b) Inserting a reference electrode into the reference electrode socket;
c) Polishing the working electrode with polishing solution containing alumina powder, soaking in alkaline cleaning solution containing sodium hydroxide, cleaning and inserting into a working electrode socket;
d) The inserted three-electrode system is washed cleanly by deionized water, a measuring module is connected with a heavy metal tester, the heavy metal tester is connected with a PC end, and the whole system passage is ensured;
e) Taking 3 clean measuring cups, marking the cups as blank samples, standard samples and samples to be measured, adding electrolyte into the 3 cups, respectively adding deionized water, cobalt standard solution and water sample to be measured, and uniformly mixing for later use;
f) Entering on-line software, creating a cobalt determination project, and setting detection parameters as follows;
g) After parameters are set, a blank sample measuring cup is clamped into a measuring base, a three-electrode system is inserted into the measuring cup, the lower end of an electrode is guaranteed to be immersed into electrolyte, a PC end blank sample is clicked to start measuring the blank sample, and after the blank sample is measured, the measurement of a standard sample and a sample to be measured is sequentially carried out similarly;
h) After the measurement of the sample to be measured is completed, checking a volt-ampere curve graph, recording a potential interval of a cobalt dissolution peak of the standard sample, and calculating the concentration of cobalt element in the sample to be measured.
By adopting the technical scheme, the three-electrode system is adopted to detect cobalt element in the technical scheme, the system not only has larger Faraday current, but also has extremely small thickness of a diffusion layer around the electrode, so that the Faraday current and convection effect are separated, and the system has relatively stable mass transfer coefficient, and in dissolution analysis, errors caused by electrolyte disturbance factors and the like are avoided, so that the current is greatly proportional to the ion concentration of the solution to be detected, the cobalt element detection method has good linearity, and the accuracy of the cobalt element detection method is improved. Meanwhile, the silver/silver chloride reference electrode can provide a stable reference potential, and saturated potassium chloride in the electrode is used as a salt bridge, so that the liquid connection potential can be eliminated or reduced; the problems of zigzag dissolution peak and the like in the volt-ampere curve caused by concentration polarization can be solved through a certain processing means, so that the stability of a measurement result can be effectively improved, and the precision of a detection method is improved.
Preferably, the detection parameters are: stirring potential (mV): -2500 to-1000; stirring time(s): 5-30; enrichment potential (mV): -2500 to-1000; enrichment time(s): 5-300 parts; static potential (mV): -2500 to-1000; standing time(s): 5 to 60; scan initiation potential (mV): -1300 to-900; scan termination potential (mV): 300-800; scan rate (mV/s): 500-1000; cleaning potential (mV): 800-1500; cleaning time(s): 10 to 60; sensitivity: 1.0X10 -4 。
Through adopting above-mentioned technical scheme, optimized the testing parameter in the cobalt element detects among the this application technical scheme, suitable testing parameter for testing result is more accurate and stability preferred.
Preferably, the working electrode is selected from any one of a glassy carbon electrode, a suspended mercury electrode or a carbon paste electrode.
Preferably, the working electrode is a glassy carbon electrode.
Through adopting above-mentioned technical scheme, the glassy carbon electrode of preferred among the technical scheme of this application is as working electrode, and the glassy carbon electrode has better conductivity and chemical stability, and its coefficient of thermal expansion is little, and the texture is hard and the gas tightness is good, and life is longer. The method is important to be capable of being manufactured in batches, low in cost and capable of meeting the requirement of commercial mass production. The suspended mercury electrode is high in price, has certain toxicity, is not easy to manufacture in batches, is easy to oxidize in the use process, and is easy to cause poor reproducibility of test results. Although the carbon paste electrode has higher electrode surface decoration property, excellent electrochemical window and low raw material cost, the proportion of the adhesive is difficult to control in the manufacturing process, and the sensitivity is reduced due to too much consumption; too little can lead to poor connection between graphite particles, resulting in increased resistance and similarly affecting sensitivity. The consumption is small, and the cost of raw materials of the adhesive with good bonding effect is multiplied. In addition, the service life of the carbon paste electrode is also inferior to that of a glassy carbon electrode, and the consistency of the prepared carbon paste electrode is poor, so that the consistency and the accuracy of a measurement result are easily poor.
In summary, the present application has the following beneficial effects:
1. since the application preferably adopts the combination of ammonium chloride and ammonia water as electrolyte, NH is formed 3 -NH 4 The Cl buffer system enables cobalt element to show an anode dissolution peak on the voltammetric graph under the action of an external electric field and under specific electrochemical parameters, so that the content of the cobalt element is conveniently calculated. Ammonium chloride has certain influence on the dissolution peak of cobalt element, and can be used as supporting electrolyte, so that the potential difference of the dissolution peak of each ion becomes large, the sharpness of the peak is improved, and the sensitivity of monitoring cobalt element is improved.
2. In the application, ammonium fluoride is preferable as an additive, and the ammonium fluoride not only contains fluoride ions, but also contains ammonium ions, so that other metal ions in a sample can be effectively combined, and interference peaks are eliminated. Meanwhile, as the ammonia water in the high-concentration ammonia-ammonium chloride electrolyte is relatively volatile, the concentration of ammonium ions in the electrolyte is reduced, namely the conductive effect of the electrolyte is poor, and the ammonium ions in the electrolyte can be supplemented through the addition of ammonium fluoride, so that the concentration stability of the ammonium ions in the electrolyte is maintained, and the accuracy, stability and sensitivity of cobalt element detection are kept at higher levels.
3. According to the detection method, the cobalt element is detected through the three-electrode system, errors caused by electrolyte disturbance factors and the like are avoided in the dissolution analysis of the three-electrode system, so that the current is greatly proportional to the ion concentration of the solution to be detected, the detection method of the cobalt element has good linearity, and the accuracy of the detection method of the cobalt element is improved. And the reference voltage can be kept stable, the liquid connection potential can be eliminated or reduced, the stability of a measurement result can be effectively improved, and the precision of the detection method is improved.
4. The glassy carbon electrode is used as a working electrode, has good reproducibility and stability, can be manufactured in batches, is low in cost, and can obtain test results with good consistency, repeatability and stability.
Drawings
FIG. 1 is a plot of the voltammogram of sample a in example 1 of the present application;
FIG. 2 is a plot of the voltammogram of sample b in example 1 of the present application;
FIG. 3 is a plot of the voltammogram of sample c in example 1 of the present application;
FIG. 4 is a voltammogram of sample d in example 1 of the present application.
Detailed Description
The present application is described in further detail below with reference to examples.
In the embodiment of the present application, the selected instruments and devices are shown below, but not limited to:
medicine and instrumentation: the reagents used in the method and the subsequent examples are all analytically pure (AR), and the equipment used is a Nanotek 2000 portable heavy metal determination solution provided by Shenzhen Langshi scientific instruments, inc., mainly comprising: three electrode system (glassy carbon electrode, silver/silver chloride reference electrode and platinum counter electrode) measuring module, hand-held heavy metal tester and PC end on-line software.
Examples
Example 1
In one aspect, the application provides an electrolyte for detecting cobalt element by anodic stripping voltammetry, which comprises 0.5mol/L ammonium chloride, 30mL/L concentrated ammonia water and 45g/L ammonium fluoride, wherein the mass fraction of the concentrated ammonia water is 26%.
In another aspect, the present application provides a method for detecting cobalt element, including the steps of: the method comprises the following steps:
a) Inserting a platinum counter electrode into the counter electrode socket;
b) Inserting a silver/silver chloride reference electrode into the reference electrode socket;
c) Polishing the glassy carbon electrode with polishing solution containing alumina powder, soaking in alkaline cleaning solution containing sodium hydroxide (1 mol/L), and inserting into a working electrode socket after cleaning;
d) The inserted three-electrode system is washed cleanly by deionized water, a measuring module is connected with a heavy metal tester, the heavy metal tester is connected with a PC end, and the whole system passage is ensured;
e) Taking a clean measuring cup, marking the clean measuring cup as a blank sample, a standard sample and a sample to be measured, adding electrolyte into the cup, respectively adding deionized water, a cobalt standard solution and the sample to be measured, and uniformly mixing for later use;
the 4 clean measuring cups were filled with liquid as follows:
sample a:10mL deionized water+10 mL cobalt standard solution (1 mg/L);
sample b:10mL of cobalt electrolyte (0.5 mol/L ammonium chloride, 30mL/L concentrated ammonia) +10mL of deionized water;
sample c:10mL of cobalt electrolyte (0.5 mol/L ammonium chloride, 30mL/L concentrated ammonia) +10mL of cobalt standard solution (1 mg/L); sample d:10mL of cobalt electrolyte (0.5 mol/L ammonium chloride, 30mL/L concentrated ammonia) +10mL of cobalt standard solution (1 mg/L) +0.1mL of cobalt additive (45 g/L ammonium fluoride);
f) Entering on-line software, creating a cobalt determination project, and setting detection parameters as follows:
stirring potential (mV): -2200;
stirring time(s): 17;
enrichment potential (mV): -2200;
enrichment time(s): 10;
static potential (mV): -2200;
standing time(s): 20, a step of;
scan initiation potential (mV): -1200;
scan termination potential (mV): 550;
scan rate (mV/s): 850;
cleaning potential (mV): 1100, a method for manufacturing the same;
cleaning time(s): 35;
sensitivity: 1.0X10 -4 。
G) After parameters are set, a blank sample measuring cup is clamped into a measuring base, a three-electrode system is inserted into the measuring cup, the lower end of an electrode is guaranteed to be immersed into electrolyte, a PC end blank sample is clicked to start measuring the blank sample, and after the blank sample is measured, the measurement of a standard sample and a sample to be measured is sequentially carried out similarly;
h) After the measurement of the sample to be measured is completed, checking a volt-ampere curve graph, recording a potential interval of a cobalt dissolution peak of the standard sample, and calculating the concentration of cobalt element in the sample to be measured.
7 cobalt standard solutions with the concentration of 0.4mg/L are prepared according to the liquid adding mode of the sample d to be used as samples 1 to 7. Selecting an area method, wherein the integral window interval is-750 mV to-50 mV, continuously measuring one sample for 6 times according to the method, recording the measured concentration each time and calculating the measurement precision (namely Relative Standard Deviation (RSD)), wherein the specific numerical values refer to table 1; the concentrations of 7 replicates, i.e. samples 1 to 7, were then measured and recorded in sequence, and the error in the indication calculated, for specific values, see table 2.
Table 1 example 1 sample test results
TABLE 2 test results for samples 1-7 in example 1
Example 2
The difference from example 1 is that: the enrichment time was set to 300s, and 6 cobalt standard solutions with a concentration of 0.01mg/L were prepared as samples 8 to 13 in the manner of adding the liquid to sample d in example 1. The "area method" was selected, the integration window interval was-750 to-50 mV, the concentrations of samples 8 to 13 were tested, and the detection limit was calculated, with specific data being referred to in Table 3.
TABLE 2 test results for samples 8-13 in example 2
Example 3
In one aspect, the application provides an electrolyte for detecting cobalt element by anodic stripping voltammetry, which comprises 0.1mol/L ammonium chloride, 7mL/L concentrated ammonia water and 20g/L ammonium fluoride, wherein the mass fraction of the concentrated ammonia water is 25%.
In another aspect, the present application provides a method for detecting cobalt element, including the steps of: the method comprises the following steps:
a) Inserting a platinum counter electrode into the counter electrode socket;
b) Inserting a silver/silver chloride reference electrode into the reference electrode socket;
c) Polishing the glassy carbon electrode with polishing solution containing alumina powder, soaking in alkaline cleaning solution containing sodium hydroxide (1 mol/L), and inserting into a working electrode socket after cleaning;
d) The inserted three-electrode system is washed cleanly by deionized water, a measuring module is connected with a heavy metal tester, the heavy metal tester is connected with a PC end, and the whole system passage is ensured;
e) Taking a clean measuring cup, marking the clean measuring cup as a blank sample, a standard sample and a sample to be measured, adding electrolyte into the cup, respectively adding deionized water, a cobalt standard solution and the sample to be measured, and uniformly mixing for later use;
f) Entering on-line software, creating a cobalt determination project, and setting detection parameters as follows:
stirring potential (mV): -1000;
stirring time(s): 30;
enrichment potential (mV): -1000;
enrichment time(s): 300;
static potential (mV): -1000;
standing time(s): 60;
scan initiation potential (mV): -900;
scan termination potential (mV): 800;
scan rate (mV/s): 500;
cleaning potential (mV): 800;
cleaning time(s): 10;
sensitivity: 1.0X10 -4 。
G) After parameters are set, a blank sample measuring cup is clamped into a measuring base, a three-electrode system is inserted into the measuring cup, the lower end of an electrode is guaranteed to be immersed into electrolyte, a PC end blank sample is clicked to start measuring the blank sample, and after the blank sample is measured, the measurement of a standard sample and a sample to be measured is sequentially carried out similarly;
h) After the measurement of the sample to be measured is completed, checking a volt-ampere curve graph, recording a potential interval of a cobalt dissolution peak of the standard sample, and calculating the concentration of cobalt element in the sample to be measured.
Sample d:10mL of cobalt electrolyte (0.1 mol/L ammonium chloride, 7mL/L concentrated ammonia) +10mL of cobalt standard solution (1 mg/L) +0.1mL of cobalt additive (20 g/L ammonium fluoride);
7 cobalt standard solutions with the concentration of 0.4mg/L are prepared according to the liquid adding mode of the sample d to be used as samples 1 to 7. Selecting an area method, wherein the integral window interval is-750 mV to-50 mV, continuously measuring one sample for 6 times according to the method, calculating the measurement precision (namely, relative Standard Deviation (RSD)), and referring to a specific numerical value in Table 4; the error of the indication is then calculated by measuring 7 replicates in sequence, for specific values, see table 4.
Example 4
In one aspect, the application provides an electrolyte for detecting cobalt element by anodic stripping voltammetry, which comprises 1mol/L ammonium chloride, 49mL/L concentrated ammonia water and 80g/L ammonium fluoride, wherein the mass fraction of the concentrated ammonia water is 28%.
In another aspect, the present application provides a method for detecting cobalt element, including the steps of: the method comprises the following steps:
a) Inserting a platinum counter electrode into the counter electrode socket;
b) Inserting a silver/silver chloride reference electrode into the reference electrode socket;
c) Polishing the glassy carbon electrode with polishing solution containing alumina powder, soaking in alkaline cleaning solution containing sodium hydroxide (1 mol/L), and inserting into a working electrode socket after cleaning;
d) The inserted three-electrode system is washed cleanly by deionized water, a measuring module is connected with a heavy metal tester, the heavy metal tester is connected with a PC end, and the whole system passage is ensured;
e) Taking a clean measuring cup, marking the clean measuring cup as a blank sample, a standard sample and a sample to be measured, adding electrolyte into the cup, respectively adding deionized water, a cobalt standard solution and the sample to be measured, and uniformly mixing for later use;
f) Entering on-line software, creating a cobalt determination project, and setting detection parameters as follows:
stirring potential (mV): -2500;
stirring time(s): 5, a step of;
enrichment potential (mV): -2500;
enrichment time(s): 5, a step of;
static potential (mV): -2500;
standing time(s): 5, a step of;
scan initiation potential (mV): -1300;
scan termination potential (mV): 800;
scan rate (mV/s): 1000;
cleaning potential (mV): 1500;
cleaning time(s): 60;
sensitivity: 1.0X10 -4 。
G) After parameters are set, a blank sample measuring cup is clamped into a measuring base, a three-electrode system is inserted into the measuring cup, the lower end of an electrode is guaranteed to be immersed into electrolyte, a PC end blank sample is clicked to start measuring the blank sample, and after the blank sample is measured, the measurement of a standard sample and a sample to be measured is sequentially carried out similarly;
h) After the measurement of the sample to be measured is completed, checking a volt-ampere curve graph, recording a potential interval of a cobalt dissolution peak of the standard sample, and calculating the concentration of cobalt element in the sample to be measured.
Sample d:10mL of cobalt electrolyte (1 mol/L ammonium chloride, 49mL/L concentrated ammonia) +10mL of cobalt standard solution (1 mg/L) +0.1mL of cobalt additive (80 g/L ammonium fluoride);
7 cobalt standard solutions with the concentration of 0.4mg/L are prepared according to the liquid adding mode of the sample d to be used as samples 1 to 7. Selecting an area method, wherein the integral window interval is-750 to-50 mV, continuously measuring the sample 1 for 6 times according to the method, calculating the measurement precision (namely, relative Standard Deviation (RSD)), and referring to a specific numerical value in Table 4; the concentrations of samples 1 to 7 were then measured sequentially to calculate the error in the indication, and the specific values are shown in Table 4.
Example 5
The difference from example 1 is that: in this example, sodium fluoride was used as an additive, the concentration of the sample was measured and the measurement precision and the error value of the indication were calculated, and the specific values are shown in table 4.
Example 6
The difference from example 1 is that: in this example, ascorbic acid was used as an additive, the concentration of the sample was measured and the measurement precision and the error value of the indication were calculated, and the specific values are shown in Table 4.
Example 7
The difference from example 1 is that: in this example, hydroxylamine hydrochloride was used as an additive, and the concentration of the sample was measured and the measurement precision and the error value of the indication were calculated, and the specific values are shown in Table 4.
Example 8
The difference from example 1 is that: in this embodiment, a mercury suspension electrode is used as a working electrode, the concentration of the sample is measured, and the measurement precision and the error value of the indication value are calculated, and the specific numerical values are referred to in table 4.
Example 9
The difference from example 1 is that: in this example, a carbon paste electrode was used as a working electrode, and the concentration of the sample was measured and the measurement precision and the error value of the indication value were calculated, and the specific values are shown in table 4.
Comparative example
Comparative example 1
The difference between this comparative example and example 1 is that in this comparative example, the suspended mercury electrode was used in combination with the ammonium chloride-dimethylglyoxime system electrolyte instead of the electrolyte and working electrode in example 1, the sample was tested, and the measurement precision and indication error value were calculated, and the specific numerical values were as shown in table 4.
Comparative example 2
The difference between this comparative example and example 1 is that the glassy carbon electrode is used in combination with the sodium hydroxide-5-Br-PADAP system electrolyte in place of the electrolyte and working electrode in example 1, the sample is tested, the measurement precision and the indication error value are calculated, and the specific numerical values are shown in Table 4.
Comparative example 3
The comparative example is different from example 1 in that the carbon paste electrode is utilized to be matched with the ammonium chloride-phenanthroline system electrolyte to replace the electrolyte and the working electrode in example 1, the sample is detected, the measurement precision and the indication error value are calculated, and the specific numerical values are shown in table 4.
Comparative example 4
The difference between this comparative example and example 1 is that the sodium nitrate electrolyte was used in place of the electrolyte in example 1 to calculate the measurement precision and the indication error value, and the specific numerical values are shown in table 4.
TABLE 4 detection results for examples 1, 3-9, comparative examples 1-4
Comparison of the test results in connection with FIGS. 1-4 and Table 4 shows that:
as can be seen from comparison of fig. 1 to 3, under the corresponding detection method, the electrolyte configured by the technical scheme of the application can indeed cause an obvious dissolution peak on the voltammogram of cobalt, but at the same time has an interference peak beside the dissolution peak; as can be seen from fig. 3 and 4, the addition of the additive eliminates the interference peak to some extent. Due to addition ofThe agent contains fluoride ion (F) - ) And ammonium ion (NH) 4 + ) These two common ligands can mask these interfering factors; at the same time high concentration of NH 4 + And part of loss of the electrolyte caused by volatilization of the ammonia water can be supplemented, so that the accuracy of a test result is improved synergistically.
(1) Comparison of examples 1, 3-4, 5-7 and comparative examples 1-4 shows that: the results of the tests obtained in example 1 and examples 3 to 5 have smaller precision and indication errors, which means that the present application forms NH by combining ammonium chloride and strong ammonia as electrolyte 3 -NH 4 The Cl buffer system enables cobalt element to show an anode dissolution peak on the voltammetric graph under the action of an external electric field and under specific electrochemical parameters, so that the content of the cobalt element is conveniently calculated. The ammonium chloride can be used as a supporting electrolyte, so that the potential difference of each ion elution peak is increased, the sharpness of the peak is improved, and the sensitivity of cobalt element monitoring is improved. The addition of ammonium fluoride not only eliminates interference peaks through the reaction of fluoride ions and other metal ions; the concentration of ammonium ions in the electrolyte can be supplemented, the stability of the electrolyte is maintained, and the accuracy of the detection result is synergistically improved.
(2) Comparison of examples 1, examples 8-9 and comparative examples 1-4 shows that: the detection results obtained in examples 8-9 have larger precision and indication error, which indicates that the glassy carbon electrode is selected as a working electrode, and has better conductivity and chemical stability, small thermal expansion coefficient, hard texture, good air tightness and longer service life. The method has the advantages of mass production, low cost, capability of meeting the requirement of commercial mass production, and capability of obtaining test results with better consistency, repeatability and stability. The mercury suspension electrode or the carbon paste electrode is easy to cause poor reproducibility of the test result and has the defect of poor consistency of finished products, so that the precision and the indication error of the detection result of the cobalt element are larger.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (10)
1. An electrolyte for detecting cobalt element by an anodic stripping voltammetry method is characterized by comprising the following substances: 0.1-1 mol/L ammonium chloride, 20-80 g/L additive and 7-49 mL/L concentrated ammonia water.
2. The electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 1, which is characterized in that: the additive is selected from any one or more of fluoride, amine compounds or organic acid.
3. The electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 2, which is characterized in that: the fluoride is selected from any one of sodium fluoride, potassium fluoride, ammonium fluoride and ammonium bifluoride.
4. The electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 2, which is characterized in that: the amine compound is selected from triethanolamine or hydroxylamine hydrochloride.
5. The electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 2, which is characterized in that: the organic acid is selected from any one of ascorbic acid, citric acid, oxalic acid or glycine.
6. An electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 3, which is characterized in that: the fluoride is ammonium fluoride.
7. The electrolyte for detecting cobalt element by an anodic stripping voltammetry according to claim 5, which is characterized in that: is prepared from the following substances in percentage by weight: 0.5mol/L ammonium chloride, 30mL/L concentrated ammonia water and 45g/L ammonium fluoride.
8. A cobalt element detection method is characterized in that: an electrolyte for detecting cobalt element by using the anodic stripping voltammetry according to any one of claims 1-7, comprising the following steps:
a) Inserting a platinum counter electrode into the counter electrode socket;
b) Inserting a silver/silver chloride reference electrode into the reference electrode socket;
c) Polishing the working electrode with polishing solution containing alumina powder, soaking in alkaline cleaning solution containing sodium hydroxide, cleaning and inserting into a working electrode socket;
d) The inserted three-electrode system is washed cleanly by deionized water, a measuring module is connected with a heavy metal tester, the heavy metal tester is connected with a PC end, and the whole system passage is ensured;
e) Taking 3 clean measuring cups, marking the cups as blank samples, standard samples and samples to be measured, adding electrolyte into the 3 cups, respectively adding deionized water, cobalt standard solution and water sample to be measured, and uniformly mixing for later use;
f) Entering on-line software, creating a cobalt determination project, and setting detection parameters as follows;
g) After parameters are set, a blank sample measuring cup is clamped into a measuring base, a three-electrode system is inserted into the measuring cup, the lower end of an electrode is guaranteed to be immersed into electrolyte, a PC end blank sample is clicked to start measuring the blank sample, and after the blank sample is measured, the measurement of a standard sample and a sample to be measured is sequentially carried out similarly;
h) After the measurement of the sample to be measured is completed, checking a volt-ampere curve graph, recording a potential interval of a cobalt dissolution peak of the standard sample, and calculating the concentration of cobalt element in the sample to be measured.
9. The method for detecting cobalt element according to claim 8, wherein: the detection parameters are as follows:
stirring potential (mV): -2500 to-1000;
stirring time(s): 5-30;
enrichment potential (mV): -2500 to-1000;
enrichment time(s): 5-300 parts;
static potential (mV): -2500 to-1000;
standing time(s): 5 to 60;
scan initiation potential (mV): -1300 to-900;
scan termination potential (mV): 300-800;
scan rate (mV/s): 500-1000;
cleaning potential (mV): 800-1500;
cleaning time(s): 10 to 60;
sensitivity: 1.0 X 10 -4 。
10. The method for detecting cobalt element according to claim 8, wherein: the working electrode is selected from any one of a glassy carbon electrode, a mercury suspension electrode or a carbon paste electrode.
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