CN112285041B - Rapid detection method for ionic liquid content - Google Patents
Rapid detection method for ionic liquid content Download PDFInfo
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- CN112285041B CN112285041B CN202011061462.6A CN202011061462A CN112285041B CN 112285041 B CN112285041 B CN 112285041B CN 202011061462 A CN202011061462 A CN 202011061462A CN 112285041 B CN112285041 B CN 112285041B
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Abstract
The invention discloses a rapid detection method for ionic liquid content, and belongs to the field of analysis and detection. The detection reagent is prepared from sodium tungstate, 85% phosphoric acid and concentrated hydrochloric acid, a working curve is based on 1-butyl-3-methylimidazolium tetrafluoroborate, 4mL of ionic liquid with different concentrations reacts with 1mL of the detection reagent, and then the light absorption value is detected at the wavelength of 600nm, so that the working curve is prepared. And (3) after the pretreated supernatant of the water body or soil sample reacts with the detection reagent, measuring the absorbance of the system, and obtaining the ionic liquid content in the sample according to the working curve and the dilution multiple. The detection reagent used by the method is convenient to prepare, cheap and easy to obtain, the instrument is common, the detection reaction time is short, the result is obvious, and the method can provide quick, simple and economic quantitative determination for quality inspection departments and production enterprises.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a rapid detection method for ionic liquid content.
Background
The ionic liquid is salt completely composed of organic positive ions and inorganic or organic negative ions and is in a liquid state at room temperature or near room temperature, has the advantages of good thermal stability, low vapor pressure, no color, no odor, difficult volatilization and the like, and shows good solubility on inorganic substances, organic substances and high polymer materials. Based on different anion and cation compositions, the types of anions and cations in the ionic liquid can be adjusted according to needs to change the properties of the ionic liquid so as to meet various practical application needs. Compared with the conventional organic solvent, the ionic liquid has lower direct harm and can be recycled, so the ionic liquid is known as a green solvent.
As a novel green solvent capable of replacing volatile organic solvents, the ionic liquid is widely applied to the fields of extraction, organic matter synthesis, catalysis, analytical chemistry and the like. However, from an environmental point of view, ionic liquids are not truly green products. Research shows that the ionic liquid has potential toxicity. During the process of synthesizing and applying ionic liquid in large quantity, the ionic liquid is inevitably released to the environment, which is not beneficial to the ecological environment. Therefore, the establishment of an efficient and accurate analysis method for the ionic liquid content in the environment is of great significance, and a basis is provided for correctly evaluating the influence of the ionic liquid on the environment.
The traditional ionic liquid detection method mainly comprises a chromatography method, a thermogravimetric analysis method, an ultraviolet spectroscopy method and the like. However, various detection methods have their drawbacks. The chromatography operation is complex, the instrument is expensive, and the analysis cost is high; the thermogravimetric analysis requires a long time and cannot be applied to conventional rapid analysis; the ultraviolet spectroscopy has a plurality of influencing factors, is suitable for pure ionic liquid and is not suitable for a mixture sample containing other compounds with absorption in an ultraviolet region. Therefore, it is necessary to develop a cheap, rapid and convenient method for detecting the content of the ionic liquid.
Disclosure of Invention
The invention aims to provide a method for quickly, conveniently and accurately detecting the content of ionic liquid in a sample aiming at the defects of the prior art. Specifically, quantitative analysis is carried out on various ionic liquids containing imidazole type cations in water or soil.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for rapidly detecting the content of ionic liquid comprises the following steps:
(1) Preparation of a detection reagent: weighing 10g of sodium tungstate, adding 5mL of 85% (mass concentration) phosphoric acid, adding 10mL of concentrated hydrochloric acid, heating to dissolve, and then dissolving in 100mL of water;
(2) Making a working curve: dissolving 1-butyl-3-methylimidazolium tetrafluoroborate in water, respectively taking 4mL of the ionic liquid with the concentration of 0-200 mug/mL into a test tube, adding 1mL of a detection reagent, reacting at 25 ℃ for 6-10 min, and detecting the light absorption value at the wavelength of 600 nm. Taking the concentration of the ionic liquid as a horizontal coordinate and the light absorption value as a vertical coordinate to obtain a working curve;
(3) Collecting and pretreating a sample: collecting water samples or soil to be detected, and respectively adopting the following methods to carry out pretreatment;
water body sample: putting 10mL of water sample into a centrifuge tube, centrifuging at 4000rpm for 10min, and collecting supernatant;
soil sample: weighing 1g of soil, adding 10mL of distilled water, fully shaking and mixing 30min, centrifuging at 5000rpm for 20min, and collecting supernatant;
(4) Analysis and determination: diluting the treatment solution in the step (3) by a certain multiple, mixing 4mL of a diluted sample with 1mL of the detection reagent in the step (1), reacting at 25 ℃ for 6-10 min, detecting an absorbance value at a wavelength of 600nm, and obtaining the ionic liquid content in the sample according to a working curve and the dilution multiple.
Compared with the prior art, the invention has the following advantages:
1. the detection reagent for analyzing the content of the ionic liquid is convenient to prepare, low in price and easy to obtain;
2. instruments required by analysis and detection are common and low in price;
3. the method has the advantages of short detection reaction time, obvious result and low detection cost, and can provide quick, simple and economic quantitative determination for quality inspection departments and production enterprises.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the invention are not limited thereto.
Example 1 analysis of tap Water samples with Ionic liquid standards Using this method
(1) Preparation of a detection reagent: weighing 10g of sodium tungstate, adding 5mL of 85% (mass concentration) phosphoric acid, adding 10mL of concentrated hydrochloric acid, heating to dissolve, and then dissolving in 100mL of water;
(2) Making a working curve: dissolving 1-butyl-3-methylimidazolium tetrafluoroborate in water, respectively taking 4mL of the ionic liquid with the concentration of 0-200 mug/mL into a test tube, adding 1mL of a detection reagent, reacting at 25 ℃ for 6-10 min, and detecting the light absorption value at the wavelength of 600 nm. And (4) taking the concentration of the ionic liquid as a horizontal coordinate and the light absorption value as a vertical coordinate to obtain a working curve.
(3) Collecting and pretreating a sample: taking six parts of tap water with the volume of 10mL, respectively adding ionic liquids of 1-butyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole chloride and 1-butyl-2.3-dimethylimidazole chloride with final concentrations of 100 mu g/mL and 500 mu g/mL, centrifuging at 4000rpm for 10min, and collecting the supernatant;
(4) Analysis and determination: diluting the supernatant in the step (3) by a certain multiple, mixing 4mL of the diluted sample with 1mL of the detection reagent in the step (1), reacting at 25 ℃ for 6-10 min, detecting the light absorption value at the wavelength of 600nm, and obtaining the ionic liquid content in the sample according to the working curve and the dilution multiple. The results are shown in Table 1. As can be seen from Table 1, the recovery rates of various ionic liquids in tap water are between 95% and 110%, and the detection requirements are met.
TABLE 1 recovery of ionic liquids from tap water using a standard addition
Example 2 analysis of soil samples with ionic liquid standards by this method
(1) Preparation of a detection reagent: weighing 10g of sodium tungstate, adding 5mL of 85% phosphoric acid, adding 10mL of concentrated hydrochloric acid, heating to dissolve, and then dissolving in 100mL of water;
(2) Making a working curve: dissolving 1-butyl-3-methylimidazole tetrafluoroborate in water by taking as a standard, respectively taking 4mL of the ionic liquid with the concentration of 0-200 mu g/mL into a test tube, adding 1mL of a detection reagent, reacting at 25 ℃ for 6-10 min, and detecting a light absorption value at the wavelength of 600 nm. And (4) taking the concentration of the ionic liquid as a horizontal coordinate and the light absorption value as a vertical coordinate to obtain a working curve.
(3) Collecting and pretreating a sample: taking six parts of soil with the mass of 1g, adding 10mL of distilled water respectively, adding 100 mu g/mL and 500 mu g/mL of ionic liquids of 1-butyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium chloride and 1-butyl-2.3-dimethylimidazolium chloride respectively, fully shaking and mixing for 30min, centrifuging at 5000rpm for 20min, and collecting supernate;
(4) Analysis and determination: diluting the supernatant in the step (3) by a certain multiple, mixing 4mL of a diluted sample with 1mL of the detection reagent in the step (1), reacting at 25 ℃ for 6-10 min, detecting the light absorption value at the wavelength of 600nm, and obtaining the ionic liquid content in the sample according to a standard curve and the dilution multiple. The results are shown in Table 2. As can be seen from Table 2, the standard recovery rates of various ionic liquids in the soil are between 95% and 110%, and the detection requirements are met.
TABLE 2 recovery of ionic liquids in soil with spiking
Claims (1)
1. A rapid detection method for ionic liquid content is characterized by comprising the following steps:
(1) Preparation of a detection reagent: weighing 10g of sodium tungstate, adding 5mL of phosphoric acid with the mass concentration of 85%, adding 10mL of concentrated hydrochloric acid, heating for dissolving, and then dissolving in 100mL of water;
(2) Making a working curve: dissolving 1-butyl-3-methylimidazole tetrafluoroborate serving as a standard in water, respectively taking 4mL of the ionic liquid with the concentration of 0-200 mug/mL into a test tube, adding 1mL of a detection reagent, reacting at 25 ℃ for 6-10 min, and detecting a light absorption value at the wavelength of 600 nm; taking the concentration of the ionic liquid as an abscissa and the light absorption value as an ordinate to obtain a working curve;
(3) Collecting and pretreating a sample: collecting water samples or soil to be detected, and respectively adopting the following methods for pretreatment;
water body sample: putting 10mL of water sample into a centrifuge tube, centrifuging at 4000rpm for 10min, and collecting supernatant;
soil sample: weighing 1g of soil, adding 10mL of distilled water, fully shaking and mixing 30min, centrifuging at 5000rpm for 20min, and collecting supernatant;
(4) Analysis and determination: diluting the treatment solution in the step (3) by a certain multiple, mixing 4mL of a diluted sample with 1mL of the detection reagent in the step (1), reacting at 25 ℃ for 6-10 min, detecting an absorbance value at a wavelength of 600nm, and obtaining the ionic liquid content in the sample according to a working curve and the dilution multiple;
the detection reagent in the step (1) consists of sodium tungstate, phosphoric acid and concentrated hydrochloric acid, wherein the concentration of sodium tungstate is 10g, the concentration of 85% phosphoric acid is 5mL, and the concentration of concentrated hydrochloric acid is 10mL;
the working curve in the step (2) is obtained by taking 1-butyl-3-methylimidazole tetrafluoroborate as a standard and reacting with a detection reagent;
the analytical assay described in step (4) is a reaction of the sample with the detection reagent according to a ratio of 4:1, and reacting for 6-10 min at 25 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101661002A (en) * | 2009-09-25 | 2010-03-03 | 福建农林大学 | Reagent for determining total phenol in water, preparation method and use thereof |
| CN103293119A (en) * | 2013-05-24 | 2013-09-11 | 淮海工学院 | Method for rapidly detecting contents of amaranthus red and brilliant blue in foods |
| CN104280491A (en) * | 2013-07-04 | 2015-01-14 | 新疆农垦科学院 | Analysis method for detecting 11 ionic liquid cations in soil |
| CN107300531A (en) * | 2017-07-01 | 2017-10-27 | 中国科学院兰州化学物理研究所 | The detection method of N methylimidazoles content in a kind of glyoxaline ion liquid |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101661002A (en) * | 2009-09-25 | 2010-03-03 | 福建农林大学 | Reagent for determining total phenol in water, preparation method and use thereof |
| CN103293119A (en) * | 2013-05-24 | 2013-09-11 | 淮海工学院 | Method for rapidly detecting contents of amaranthus red and brilliant blue in foods |
| CN104280491A (en) * | 2013-07-04 | 2015-01-14 | 新疆农垦科学院 | Analysis method for detecting 11 ionic liquid cations in soil |
| CN107300531A (en) * | 2017-07-01 | 2017-10-27 | 中国科学院兰州化学物理研究所 | The detection method of N methylimidazoles content in a kind of glyoxaline ion liquid |
Non-Patent Citations (1)
| Title |
|---|
| 酱油中4-甲基咪唑含量测定方法的研究;赵俊平 等;《中国酿造》;20101231;全文 * |
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