CN114002174B - Ultraviolet absorption spectrometry for accurately measuring silver ion content - Google Patents

Ultraviolet absorption spectrometry for accurately measuring silver ion content Download PDF

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CN114002174B
CN114002174B CN202111130771.9A CN202111130771A CN114002174B CN 114002174 B CN114002174 B CN 114002174B CN 202111130771 A CN202111130771 A CN 202111130771A CN 114002174 B CN114002174 B CN 114002174B
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silver ion
solution
silver
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ionic liquid
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CN114002174A (en
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刘琦
杨婷
闫兵
张丽
宋婷
贺小琴
郑燕
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Shaanxi New Era Biotransformation Detection Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

The application relates to the field of silver ion detection methods, and particularly discloses an ultraviolet absorption spectrometry for accurately measuring silver ion content, which comprises the steps of preparing a silver ion standard detection solution, drawing a standard curve and silver ion detection, wherein a sufficient amount of nitric acid solution, p-phenylenediamine and ionic liquid containing heteroatom rings are added into a test sample, the p-phenylenediamine and the ionic liquid containing heteroatom rings can selectively adsorb silver ions in the test sample under the combined action of the p-phenylenediamine and the ionic liquid containing heteroatom rings, then the silver ions are extracted by an organic solvent, finally the solvent is evaporated to dryness and then the volume is fixed, and ultraviolet absorption measurement is carried out, so that the concentration of silver ions in waste liquid can be accurately measured by the test method, and the ultraviolet detection method is convenient and efficient.

Description

Ultraviolet absorption spectrometry for accurately measuring silver ion content
Technical Field
The application relates to the field of silver ion detection methods, in particular to an ultraviolet absorption spectrometry for accurately measuring silver ion content.
Background
Silver is widely applied in industries such as electronics, electroplating, sensitization and the like, so that a large amount of silver ions are generated in industrial wastewater, and the silver of the silver ions has high toxicity, seriously pollutes the environment and endangers the health of people. Currently, the World Health Organization (WHO) recommends a maximum concentration of 0.1ppm allowed in drinking water, and therefore, the detection of silver ions is significant for protecting the environment and maintaining the physical health of people.
At present, a common silver ion detection method is a flame atomic absorption spectrometry, and a gaseous atom can absorb light radiation with a certain wavelength, so that electrons in the outer layer of the atom are transited from a ground state to an excited state, radiation light with a certain wavelength is selectively resonantly absorbed, the incident light is weakened, the degree of weakening of a characteristic spectral line of the atom due to absorption is called absorbance, and the absorbance is in direct proportion to the content of a detected element in a linear range.
The related art has the defects that a large amount of other metal ions exist in industrial wastewater, and if the detection is directly performed by a flame atomic absorption spectrometry, the interference is large, so that the silver ion measurement is inaccurate.
Disclosure of Invention
In order to accurately detect the content of silver ions, the application provides an ultraviolet absorption spectrometry for accurately measuring the content of silver ions.
The application provides an ultraviolet absorption spectrometry for accurately measuring silver ion content, which adopts the following technical scheme: an ultraviolet absorption spectrometry for accurately measuring silver ion content comprises the following steps,
(1) Preparing a silver ion standard detection solution: adding water into a silver nitrate standard substance to prepare a silver ion solution, adding p-phenylenediamine and an ionic liquid containing a heteroatom ring into the silver ion solution, stirring, adding an organic solvent to extract, separating an organic phase, namely the silver ion standard solution, evaporating the silver ion standard solution, adding the organic solvent to fix the volume to different volumes to obtain silver ion standard detection solutions with different concentrations, wherein the mass ratio of the p-phenylenediamine to the ionic liquid is (3-5): 1, a step of;
(2) Drawing a standard curve: carrying out ultraviolet detection on the silver ion standard detection solution in the step (1), and drawing a standard curve;
(3) Silver ion detection: adding a sufficient amount of nitric acid solution into the solution to be detected to obtain a silver ion solution to be detected, taking a fixed volume of the silver ion solution to be detected, and adding p-phenylenediamine and an ionic liquid containing a heteroatom ring into the silver ion solution to be detected; stirring, adding a sufficient amount of organic solvent for extraction, evaporating an organic layer, adding the organic solvent for volume fixing to obtain a test sample, performing ultraviolet absorption spectrum detection on the test sample, substituting the measured absorbance value into the standard curve measured in the step (2) for calculation, and obtaining the concentration of the ionic solution of the test sample, wherein the mass ratio of the ionic liquid p-phenylenediamine is (3-5): 1, calculating the concentration of silver ions in the solution to be detected.
By adopting the technical scheme, silver ions in mixed ions in the waste liquid are separated and enriched, and then the enriched silver ions are detected by an ultraviolet absorption spectrometry, so that interference of other ions on detection results is reduced, the measurement results are accurate, and in addition, the ultraviolet spectrophotometer has the advantages of high analysis speed and strong operability, so that research on detecting silver ion content by the ultraviolet absorption spectrometry has potential advantages and applicable prospects.
The ultraviolet absorption spectrometry is a method for qualitatively and quantitatively analyzing substances by utilizing the absorption effect of molecules and ions of the substances on light in a certain wavelength range, so that a reagent to be detected has selective absorption on ultraviolet light, and interference of interfering substances on silver ions needs to be removed, so that the detection result of the silver ions is more accurate. The components in the wastewater are mixed and contain a plurality of precipitates, so that silver ions in the wastewater are required to be separated from other components, nitric acid solution is added into the wastewater, and nitric acid has strong oxidizing property, so that the silver components in the wastewater exist in the form of silver ions, and the detection value of the subsequent silver ions is more accurate; in addition, the nitric acid helps to clarify the whole waste liquid, further reduces the possibility that partial silver components are wrapped or complexed to influence deviation of silver ion content detection, and further helps to the accuracy of subsequent detection results.
Compared with the conventional organic solvent, the ionic liquid has the characteristics of difficult volatilization, high thermal stability, difficult environmental pollution and the like, and the ionic liquid has structural adjustability, and can generate ionic liquids with different characteristics by changing the types of anions and cations, so that the high-selectivity heteroatom-containing ring ionic liquid capable of performing a coordination function with silver ions is added into the liquid to be detected, the heteroatom-containing ring ionic liquid can adsorb silver ions in wastewater to achieve the function of separating silver ions, and the heteroatom-containing ring ionic liquid can selectively adsorb silver ions in wastewater because the heteroatom-containing ring ionic liquid is difficult to be coordinated with other metal ions, thereby being beneficial to making the measurement result of silver ions accurate.
The method comprises the steps that the heteroatom in the heteroatom-containing ring ionic liquid and cations in the wastewater generate the action between Lewis acid-base electron pairs, so that silver ions in the wastewater are adsorbed into the heteroatom-containing ring ionic liquid, then an organic solvent is added into the wastewater, and the ionic liquid with the adsorbed metal cations and the complex are less than the ionic liquid with the adsorbed silver ions in the organic solvent in solubility in water, so that the ionic liquid with the adsorbed metal cations can be extracted from an aqueous solution by the organic solvent, and when the heteroatom-containing ring ionic liquid with the selectively adsorbed silver ions is added into the wastewater, the organic solvent is added, so that the separation and enrichment of silver ions in the wastewater can be realized, other ions are not easy to mix into a silver ion detection liquid, and the detection accuracy of the silver ion content is improved.
The method for measuring the silver ion content by the standard curve method is simple and efficient, but the ultraviolet absorption luminosity value is deviated due to the fact that the trace substances can also generate ultraviolet absorption, so that when the silver ion standard detection solution is prepared, the treatment mode of the silver nitrate solution is kept consistent with the treatment mode of the silver ion solution to be measured, the influence of the ionic liquid on the silver ion content is eliminated, and the accuracy of silver ion content measurement is improved.
Optionally, the heteroatom-containing ring ionic liquid is any one of 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline.
By adopting the technical scheme, through test, the 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline can selectively adsorb silver ions, have good adsorption performance on silver ions, and can fully contact with silver ions in wastewater.
Because silver ions belong to soft acid, and N on heterocycle in 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline is soft alkali, the silver ions in the wastewater can be strongly adsorbed by the 1, 3-dimethyl imidazole hexafluorophosphate, the 1, 3-dimethyl-imidazole nitrate and the 4, 5-dimethyl-2-isobutyl thiazoline, so that an excellent separation effect is achieved; in addition, compared with other ionic liquids, the 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline have simpler structures, and after adsorbing silver ions, a branched chain is not easy to react with the silver ions or mask the silver ions; when the ultraviolet absorption spectrometry is adopted to measure the silver ions, the ultraviolet absorption peaks of the 1, 3-dimethyl imidazole hexafluorophosphate, the 1, 3-dimethyl-imidazole nitrate and the 4, 5-dimethyl-2-isobutyl thiazoline are simpler, the ultraviolet detection of the silver ions is not easy to interfere, and the accuracy of the silver ion detection is further facilitated.
Optionally, in the step (2) and in the step (3), the ultraviolet detection wavelength is 280-410nm.
By adopting the technical scheme, under the ultraviolet detection wavelength of 280-410nm, the response value of the substances coordinated by the 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline and silver ions to ultraviolet light is high, so that the quantitative detection of the silver ions is facilitated.
Optionally, the organic solvent is cyclohexane or dichloromethane.
By adopting the technical scheme, the cyclohexane and the dichloromethane have larger solubility on the ionic liquid-silver complex, which is beneficial to extraction, and the cyclohexane and the dichloromethane are symmetrical structures, and only sigma-sigma is adopted * The transition is simple, the peak shape is simple, and the absorption peak is single at 280-410nm, so that the silver ion detection peak is not easy to influence.
Optionally, in the step (1), the mass ratio of silver nitrate to the heteroatom-containing ring ionic liquid is 1: (2-3).
By adopting the technical scheme, the ionic liquid can be fully contacted with silver ions, so that the silver ions and the heteroatom-containing ring ionic liquid form a complex.
Optionally, the concentration range of the silver ion standard detection solution in the step (2) is 0.075-50ppm, and the detection quantity of the silver ion standard detection solution is 6-10 items.
By adopting the technical scheme, when the standard detection range of silver ions is 0.075-50ppm, the linear range of the concentration of silver ions and absorbance value is good, and the method is favorable for accurately calculating the concentration of the silver ion solution to be detected in the later period.
Optionally, the mixed solvent is heated after the organic solvent is added in the step (1) and the step (3), the heating temperature is 30-40 ℃, and the extraction time is 30-50min.
By adopting the technical scheme, during extraction, the extraction efficiency and effect of the organic solvent can be improved by properly heating, so that the ionic liquid complex containing silver ions enters the organic solvent, and the purpose of enrichment is achieved.
Optionally, the concentration of the nitric acid in the step (3) is 6-7mol/L.
By adopting the technical scheme, the silver components in the solution to be detected can exist in the form of silver ions, and the accuracy of silver ion detection is improved.
Optionally, the stirring mode in the step (1) and the step (3) is ultrasonic vibration.
By adopting the technical scheme, the ultrasonic vibration is favorable for fully and uniformly mixing the silver ion standard detection solution and the solution, so that the solution has uniformity, and the silver ion content is further accurately detected.
In summary, the application has the following beneficial effects:
1. complexing silver ions in the solution by adopting p-phenylenediamine and ionic liquid containing heteroatom ring, then extracting by using an organic solvent, separating and enriching the silver ions, and measuring the concentration of the silver ions by using an ultraviolet absorption spectrometry, thereby being beneficial to efficiently and accurately detecting the content of the silver ions;
2. the selective adsorption of silver ions is facilitated by using 1, 3-dimethyl imidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline, so that the purpose of effectively separating silver ions from other substances is achieved;
3. by using cyclohexane and methylene dichloride solvent, the silver-containing complex can be effectively extracted, and the ultraviolet absorption of the complex can not influence the accuracy of ultraviolet detection of silver ions.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
(1) Preparing a silver ion standard detection solution:
adding 50mg of silver nitrate standard substance into 1L of water, and fixing the volume in a 1L volumetric flask to obtain mother liquor with the concentration of 50ppm; 100mL of the mother solution is taken, 10mg of 1-butyl-3-methylimidazole hexafluorophosphate and 2mg of p-phenylenediamine are added, after ultrasonic oscillation, 150mL of dichloromethane is added, ultrasonic oscillation is carried out for 50min at the temperature of 30 ℃, after the organic phase is separated, the solvent is evaporated by a rotary evaporator, and then 100mL of dichloromethane is added to prepare a 50ppm silver ion solution.
80mL of the 50ppm silver ion solution was taken and the volume was fixed to 100mL with methylene chloride to prepare a 40ppm silver ion solution.
70mL of the 40ppm silver ion solution is taken, and methylene dichloride is adopted to fix the volume to 100mL, so that 28ppm silver ion solution is prepared.
50mL of the 28ppm silver ion solution was taken and 70mL of methylene chloride was added to prepare a 20ppm silver ion solution.
50mL of the 20ppm silver ion solution was taken and the volume was set to 100mL using methylene chloride to prepare a 10ppm silver ion solution.
50mL of the 10ppm silver ion solution was taken and the volume was adjusted to 100mL using methylene chloride to prepare a 5ppm silver ion solution.
50mL of the 10ppm silver ion solution was taken and the volume was adjusted to 100mL using methylene chloride to prepare a 2.5ppm silver ion solution.
30mL of the 2.5ppm silver ion solution was taken and the volume was adjusted to 100mL using methylene chloride to prepare a 0.75ppm silver ion solution.
10mL of the 0.75ppm silver ion solution is taken, and methylene dichloride is adopted to fix the volume to 100mL, so that 0.075ppm silver ion solution is prepared.
(2) Drawing a standard curve
And (3) measuring 5mL of the silver ion standard detection solution with each concentration obtained in the step (1) respectively, and then sequentially placing the silver ion standard detection solutions in an ultraviolet absorption photometer for detection. The absorbance at 320nm was measured at ultraviolet test wavelengths of 280-410nm by adjusting the instrument to the optimal operating conditions according to the instructions for the use of the instrument. And drawing a standard curve by taking absorbance as a response value according to the relation between the absorbance value and the concentration, wherein the linear relation is as follows: a= 0.3058X-0.0287, r 2 =0.9997, wherein a represents the absorbance value at the ultraviolet test wavelength of 320nm, and X represents the concentration of the silver ion standard solution.
(3) Silver ion detection
Accurately preparing 100mL of 2.5ppm silver nitrate solution, adding 0.11mg of nitric acid solution with the concentration of 7mol/L to obtain silver ion solution to be detected, and adding 0.5mg of 1-butyl-3-methylimidazole hexafluorophosphate and 0.1mg of p-phenylenediamine into the silver ion solution to be detected; stirring, adding 150mL of dichloromethane for extraction, carrying out ultrasonic oscillation at the temperature of 30 ℃ for 50min, separating out a machine phase, evaporating a solvent by a rotary evaporator, adding 100mL of dichloromethane to obtain a test sample, measuring 5mL of the test sample for ultraviolet absorption spectrum detection, substituting the measured absorbance value into the standard curve measured in the step (2) for calculation, and calculating the concentration of silver ions in the solution to be detected.
Example 2
(1) Preparing a silver ion standard detection solution:
the difference from example 1 is that after taking 100mL of mother liquor, 12.5mg of 1, 3-dimethyl-imidazole nitrate and 3.13mg of p-phenylenediamine are added, after ultrasonic oscillation, 150mL of cyclohexane is added, ultrasonic oscillation is carried out for 40min at 35 ℃, after separating the organic phase, the solvent is evaporated by a rotary evaporator, then 100mL of cyclohexane is added to prepare 50ppm of silver ion solution, and in the subsequent concentration configuration process, the cyclohexane is adopted;
(2) Drawing a standard curve
Operating according to step (2) of example 1, a linear relationship is obtained: a=0.3083x+0.0482, r 2 ＝0.9999。
(3) Silver ion detection
Accurately preparing 100mL of 2.5ppm silver nitrate solution, adding 0.11mg of nitric acid solution with the concentration of 6mol/L to obtain silver ion solution to be detected, and adding 0.625mg of 1-butyl-3-methylimidazole hexafluorophosphate and 0.156mg of p-phenylenediamine into the silver ion solution to be detected; after ultrasonic oscillation, 150mL of cyclohexane is added, ultrasonic oscillation is carried out for 40min at the temperature of 35 ℃, after the organic phase is separated, a rotary evaporator is used for evaporating the solvent, then 100mL of cyclohexane is added to obtain a test sample, 5mL of the test sample is measured for ultraviolet absorption spectrum detection, the measured absorbance value is substituted into the standard curve measured in the step (2) for calculation, the concentration of the ionic solution of the test sample is obtained, and the concentration of silver ions in the solution to be detected is calculated.
Example 3
(1) Preparing a silver ion standard detection solution:
the difference from preparation example 1 is that 15mg of 4, 5-dimethyl-2-isobutyl thiazoline and 5mg of p-phenylenediamine are added after 100mL of mother liquor is taken, 150mL of cyclohexane is added after ultrasonic oscillation, ultrasonic oscillation is carried out for 30min at 40 ℃, after the organic phase is separated, the solvent is evaporated by a rotary evaporator, then 100mL of cyclohexane is added again, 50ppm of silver ion solution is prepared, and the cyclohexane is adopted in the subsequent concentration configuration process.
(2) Drawing a standard curve
Operating according to step (2) of example 1, a linear relationship is obtained: a=0.3078x+0.007, r 2 ＝0.9998。
(3) Silver ion detection
Accurately preparing 100mL of 2.5ppm silver nitrate solution, adding 0.11mg of nitric acid solution with the concentration of 6.5mol/L to obtain silver ion solution to be detected, and adding 0.75mg of 1-butyl-3-methylimidazole hexafluorophosphate and 0.25mg of p-phenylenediamine; stirring, adding 150mL of dichloromethane for extraction, performing ultrasonic oscillation at the temperature of 30 ℃ for 50min, separating an organic phase, evaporating a solvent by a rotary evaporator, adding 100mL of dichloromethane to obtain a test sample, measuring 5mL of the test sample for ultraviolet absorption spectrum detection, substituting the measured absorbance value into the standard curve measured in the step (2) for calculation, and calculating the concentration of silver ions in the solution to be detected.
Example 4
The difference from example 2 is that the ionic liquid used in each step is 1-n-butyl-3-methylimidazole hexafluorophosphate.
Example 5
The difference from example 2 is that the organic solvent is not heated after the organic solvent is added in the step (1) and the step (3), and the ultrasonic vibration is directly carried out for 40min.
Example 6
The difference from example 2 is that the stirring means in step (1) and step (3) is manual stirring by a person.
Comparative example
Comparative example 1
The difference from example 2 is that no ionic liquid was added in each step.
Comparative example 2
The difference from example 2 is that no p-phenylenediamine is added in each step.
Comparative example 3
The difference from example 2 is that no ionic liquid and no p-phenylenediamine were added in each step.
Comparative example 4
The difference from example 2 is that 12.5mg of 1, 3-dimethyl-imidazole nitrate and 6mg of p-phenylenediamine are added in step (1) and step (3).
Comparative example 5
The difference from example 2 is that 12.5mg of 1, 3-dimethyl-imidazole nitrate and 1mg of p-phenylenediamine are added in step (1) and step (3).
Comparative example 6
The difference from example 2 is that in step (1) and step (3) no 1, 3-dimethyl-imidazole nitrate is added, but 12.5mg of alkyl quaternary phosphonium cation is added.
Comparative example 7
The difference from example 2 is that the nitric acid solution was not added in step (3).
Performance test
1. Accuracy detection
And (3) adopting a standard curve for quantification, substituting absorbance values in examples 1-6 and comparative examples 1-7 into corresponding standard curves in each example, and measuring the concentration of silver ions in the measured sample, so that the concentration of silver ions in the solution to be detected, which is measured by an ultraviolet absorption spectrometry in the application, can be calculated. Five measurements were made for each set of experiments to obtain the average measured concentration, the standard deviation characterizes the degree to which the measured value deviates from the true value, and the accuracy of the detection method can be characterized by the range and standard deviation, the range and standard deviation data are shown in Table 1.
Table 1.
By comparing the data of examples 1-6 and comparative examples 1-7 in Table 1, the silver ion detection method of the application is helpful for accurately measuring the concentration of silver ions, and the detection result has high accuracy and is suitable for subsequent practical application.
From the data of examples 4-6 and example 2, it is known that the type of ionic liquid and the mode of extraction with organic solvent both have an effect on the detection result of silver ions, but the accuracy is still relatively high, which indicates that the detection method of the present application is helpful for detecting silver ions.
From the data in comparative examples 1-3 and example 2, it is clear that the concentration of silver ions detected by uv absorbance photometry is not accurate when no ionic liquid or diphenylamine is added to the solution, which may be that the corresponding value of silver ions to uv is not linear without p-phenylenediamine or ionic liquid, thereby resulting in an inaccurate concentration of silver ions measured; and the concentration of silver ions measured by the method is more accurate only when the p-phenylenediamine and the ionic liquid exist simultaneously (example 2).
In addition, as is clear from the data of comparative examples 4 to 6 and comparative example 2, the ionic liquid must be an ionic liquid containing a hetero atom ring to achieve the purpose of effectively adsorbing silver ions, and the ratio of p-phenylenediamine to ionic liquid also has a great influence on the detection result of silver ions, and the concentration of silver ions can be more effectively detected only if the ratio of p-phenylenediamine to ionic liquid is in a proper range.
2. Interfering ion influence detection
1.25mg of copper sulfate, 1.25mg of ferric chloride, 1.25mg of silver nitrate, 1.25mg of nickel chloride and 1.25mg of lead chloride are added into 500mL of distilled water to prepare a mixed solution containing 2.5ppm of silver ions, then 5mg of nitric acid solution is added to obtain a silver ion solution to be detected, and then 1.88mg of 1-butyl-3-methylimidazolium hexafluorophosphate and 0.47mg of p-phenylenediamine are added into the silver ion solution; 600mL of dichloromethane is added, ultrasonic oscillation is carried out for 50min at the temperature of 30 ℃, extraction is carried out, after an organic phase is separated, a rotary evaporator is used for evaporating a solvent, 500mL of dichloromethane is added to obtain a test sample, 5mL of test sample is measured for ultraviolet absorption spectrum detection, the measured absorbance value is substituted into a standard curve measured in the embodiment 2 for calculation, the concentration of an ion solution of the test sample is obtained, and the concentration of silver ions in the solution to be detected is calculated. Average values were taken after six measurements. The concentration of silver ions in the solution to be detected was 2.487ppm and the standard deviation was 0.0071.
Therefore, the method can accurately measure the concentration of silver ions in the mixed metal ion solution, and the conclusion of the table 1 shows that the silver ion detection method is stable in detection result and high in accuracy, so that the method can be suitable for measuring the content of silver ions in wastewater, and the process of detecting silver ions by adopting an ultraviolet absorption spectrometry is simple and convenient.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.

Claims (8)

1. An ultraviolet absorption spectrometry for accurately measuring silver ion content, which is characterized in that: comprises the steps of,
(1) Preparing a silver ion standard detection solution: adding water into a silver nitrate standard substance to prepare a silver ion solution, adding p-phenylenediamine and an ionic liquid containing a heteroatom ring into the silver ion solution, stirring, adding an organic solvent to extract, separating an organic phase, namely the silver ion standard solution, evaporating the silver ion standard solution, adding the organic solvent to fix the volume to different volumes to obtain silver ion standard detection solutions with different concentrations, wherein the mass ratio of the p-phenylenediamine to the ionic liquid is (3-5): 1, a step of;
(2) Drawing a standard curve: carrying out ultraviolet detection on the silver ion standard detection solution in the step (1), and drawing a standard curve;
(3) Silver ion detection: adding a sufficient amount of nitric acid solution into the solution to be detected to obtain a silver ion solution to be detected, taking a fixed volume of the silver ion solution to be detected, and adding p-phenylenediamine and an ionic liquid containing a heteroatom ring into the silver ion solution to be detected; stirring, adding a sufficient amount of organic solvent for extraction, evaporating an organic layer, adding the organic solvent for volume fixing to obtain a test sample, performing ultraviolet absorption spectrum detection on the test sample, substituting the measured absorbance value into the standard curve measured in the step (2) for calculation, and obtaining the concentration of the ionic solution of the test sample, wherein the mass ratio of the ionic liquid p-phenylenediamine is (3-5): 1, calculating the concentration of silver ions in a solution to be detected; the concentration of the nitric acid in the step (3) is 6-7mol/L.
2. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 1, wherein: the ionic liquid containing the hetero atom is any one of 1-butyl-3-methylimidazole hexafluorophosphate, 1, 3-dimethyl-imidazole nitrate and 4, 5-dimethyl-2-isobutyl thiazoline.
3. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 2, wherein: in the step (2) and the step (3), the ultraviolet detection wavelength is 280-410nm.
4. A uv absorption spectroscopy method for accurately determining silver ion content according to any one of claims 1-3, wherein: the organic solvent is cyclohexane or dichloromethane.
5. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 1, wherein: in the step (1), the mass ratio of the silver nitrate to the heteroatom-containing ring ionic liquid is 1: (2-3).
6. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 1, wherein: the concentration range of the silver ion standard detection solution in the step (2) is 0.075-50ppm, and the number of detection items of the silver ion standard detection solution is 6-10.
7. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 1, wherein: and (3) adding an organic solvent in the step (1) and the step (3), heating the mixed solvent at the temperature of 30-40 ℃ for 30-50min.
8. An ultraviolet absorption spectrometry for accurately determining silver ion content according to claim 1, wherein: the stirring mode in the step (1) and the step (3) is ultrasonic vibration.
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