CN116242794A - Method for detecting Cr in solid agricultural product sample based on ionic liquid double water phase - Google Patents
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 26
- 239000007787 solid Substances 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002835 absorbance Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
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- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000002474 experimental method Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 235000010290 biphenyl Nutrition 0.000 claims abstract description 3
- 239000004305 biphenyl Substances 0.000 claims abstract description 3
- -1 diphenyl carbodihydrazide Chemical compound 0.000 claims abstract description 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 3
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 18
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 4
- IAZSXUOKBPGUMV-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CCCC[NH+]1CN(C)C=C1 IAZSXUOKBPGUMV-UHFFFAOYSA-N 0.000 claims description 2
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims description 2
- BZLDLXIZTKWRNF-UHFFFAOYSA-N C(C)(=O)O.C(CCCCCC)N1CN(C=C1)C Chemical compound C(C)(=O)O.C(CCCCCC)N1CN(C=C1)C BZLDLXIZTKWRNF-UHFFFAOYSA-N 0.000 claims description 2
- IJROWDLATMAXNG-UHFFFAOYSA-N C(C)(=O)O.C1(CCCCC1)CN1CN(C=C1)C Chemical compound C(C)(=O)O.C1(CCCCC1)CN1CN(C=C1)C IJROWDLATMAXNG-UHFFFAOYSA-N 0.000 claims description 2
- CUDYAOQLSZRWSH-UHFFFAOYSA-N C(C)(=O)O.C1=C(C=CC2=CC=CC=C12)CN1CN(C=C1)C Chemical compound C(C)(=O)O.C1=C(C=CC2=CC=CC=C12)CN1CN(C=C1)C CUDYAOQLSZRWSH-UHFFFAOYSA-N 0.000 claims description 2
- DETSYOQNWCXITA-UHFFFAOYSA-N C(C1=CC=CC=C1)N1CN(C=C1)C.C(C)(=O)O Chemical compound C(C1=CC=CC=C1)N1CN(C=C1)C.C(C)(=O)O DETSYOQNWCXITA-UHFFFAOYSA-N 0.000 claims description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000029087 digestion Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 244000269722 Thea sinensis Species 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 244000062793 Sorghum vulgare Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 1
- 238000002486 graphite furnace atomic emission spectrometry Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 235000019713 millet Nutrition 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012803 optimization experiment Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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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
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- 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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- 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
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Abstract
The invention discloses a method for detecting Cr in a solid agricultural product sample based on ionic liquid double water phase, which comprises the following steps: 1. preparing a chelating phase-splitting agent; 2. weighing sample powder, placing into a bottle, adding chelating phase-splitting agent, pure water and ionic liquid aqueous solution, heating in water bath to dissolve, stirring, and standing at room temperature to stabilize phase separation; 3. taking a lower phase solution, adjusting the pH value to be 2-3, completely precipitating the chelating phase-splitting agent, filtering, taking the filtered solution, putting the filtered solution into a colorimetric tube, adding an oxidant, fully reacting, adding sulfuric acid and phosphoric acid, and shaking uniformly to obtain the dye; 4. adding diphenyl carbodihydrazide solution, fixing volume with pure water, shaking, standing at room temperature, taking reagent blank as reference, performing three parallel experiments for comparison, and measuring absorbance at 540nm by ultraviolet spectrophotometry with cuvette. The invention utilizes the ionic liquid double water phase technology, the chelating phase-splitting agent is lyophile salt, separates trace Cr of agricultural products from the lower phase, and is coupled with an ultraviolet light-splitting method to establish a set of rapid detection technology for Cr in the agricultural products at normal temperature.
Description
Technical Field
The invention belongs to the technical field of heavy metal detection, and particularly relates to a method for detecting Cr in a solid agricultural product sample based on an ionic liquid double-water phase.
Background
At present, the technology for detecting Cr in a solid agricultural product sample mainly comprises an atomic absorption method and ICP, but the atomic absorption method has the defects of serious matrix interference and inapplicability to multi-element analysis. ICP operation cost is high, solid sample injection cannot be directly carried out, and advantages to some elements are not obvious. Graphite furnace and inductively coupled plasma atomic emission spectrometry are expensive, and equipment cost is high, so that the method has no possibility of popularization. And cumbersome pretreatment steps are required before GFAAS and ICP-OES analysis are performed. These two traditional methods of digestion sample preparation are cumbersome and time consuming, require the use of large amounts of hazardous reagents, generally require high temperatures, and often lead to system errors and malfunctions. In order to shorten the processing time and reduce the reagent usage, microwave-assisted digestion sampling and high-pressure digestion sampling were developed in place of these traditional sample preparation procedures. Although the two methods can accelerate sample preparation and reduce consumption of harmful reagents to a certain extent, the two methods are operated under high pressure, and have potential safety hazards. Slurry sampling has the simplest sample preparation procedure compared to digestion sampling described above, but it is difficult to maintain sample homogenization and accurate analysis. Therefore, there is an urgent need to develop a rapid, simple and safe sample preparation method for accurately measuring the chromium content in agricultural products.
Disclosure of Invention
The invention provides a method for detecting Cr in a solid agricultural product sample based on an ionic liquid double water phase, which utilizes an ionic liquid double water phase technology to separate trace Cr in the agricultural product from a lower phase by taking a synthesized chelating phase-splitting agent as a lyophile salt and establishes a set of rapid detection technology for Cr in the solid agricultural product at normal temperature by coupling an ultraviolet spectroscopic method.
The invention is realized by the following technical scheme:
the method for detecting Cr in the solid agricultural product sample based on the ionic liquid double water phase comprises the following steps:
step one, preparing a chelating phase-splitting agent;
weighing 2g of sample powder, putting the sample powder into a dry glass bottle, adding a chelating phase-splitting agent, adding pure water and 40% of ionic liquid aqueous solution, heating in a water bath at 20-30 ℃ to dissolve the sample powder, stirring the sample powder for 2-4 hours, standing the sample powder at room temperature for 30-40 min to enable the sample powder to be stable in phase separation, and separating the sample powder into an upper phase and a lower phase;
step three, taking down the phase solution, adjusting the pH value to be 2-3, completely precipitating the chelating phase-splitting agent, filtering, taking the filtered solution, placing the filtered solution into a colorimetric tube, adding the oxidant solution, fully reacting, adding 4.5mL of 1mol/L sulfuric acid solution and 0.5mL of phosphoric acid, and shaking uniformly to obtain the chelating phase-splitting agent;
and step four, adding 2.0mL of 2.5g/L diphenyl carbodihydrazide solution, fixing the volume to 50mL by using pure water, shaking uniformly, standing for 10min at room temperature, taking a reagent blank as a reference, performing three groups of parallel experiments for comparison, and measuring the absorbance at 540nm by using a 3cm cuvette through an ultraviolet spectrophotometry.
Further, in the first step, the chelating phase-splitting agent is EDTA-TBA, and the preparation method comprises the following steps: TBAH and EDTA are weighed and in aqueous solution according to TBAH: EDTA: water = 3.55: 1:50, stirring for 30min, and drying the solution in a rotary evaporator to constant weight to obtain the chelating phase-splitting agent.
Further, in the second step, the ionic liquid is at least one of tetrabutylammonium hydroxide, tetrabutylammonium chloride, tetrabutylammonium bromide, 1- (2-naphthylmethyl) -3-methylimidazole acetate, 1-heptyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate, 1-benzyl-3-methylimidazole acetate, 1- (cyclohexylmethyl) -3-methylimidazole acetate and 1-butyl-3-methylimidazole chloride.
Further, in the second step, the ionic liquid is tetrabutylammonium hydroxide.
Further, in the phase separation in the second step, the dissolved solid agricultural product sample remains in the upper phase, and Cr is separated into the lower phase.
Further, the oxidant solution in step three was 1.5mL of 100g/L potassium persulfate solution.
The invention has the beneficial effects that:
1. according to the invention, ionic liquid with special phase separation capability and chelating phase-separating agent TBA-EDTA are used for dissolving the solid agricultural product sample, and the lyophile chelating phase-separating agent is used for separating and phase-separating Cr in the dissolved solid agricultural product sample, so that the Cr is separated into an upper phase and a lower phase. Separating free Cr to a lyophile chelating phase-splitting agent enrichment phase, namely separating Cr to a lower phase, and reserving a dissolved solid agricultural product sample to an upper phase to finish separation for subsequent detection;
2. compared with the technology for detecting Cr by using an atomic absorption method and an ICP method, the technology for detecting Cr in a novel solid agricultural product sample has the advantages that expensive and large-scale detection equipment is needed in the detection process, and a plurality of limit values are caused for detection;
3. the traditional detection method requires long-time high-temperature dissolution and digestion steps, generates a large amount of acid mist, has extremely high energy consumption and is not friendly to the environment. The technical method does not need to digest the sample under extreme conditions, only dissolves and phase-separates at room temperature, so the method is friendly to the environment and the health of operators, and has great advantages;
4. the detection can be carried out without complicated sample pretreatment steps, so that the experimental operation is simplified;
5. the reagent of the method can be recycled, and the EDTA precipitate obtained after filtration and the ionic liquid of the ionic liquid enrichment phase can be recycled for subsequent recycling;
drawings
FIG. 1 is a graph showing the relationship between absorbance and reaction time in example 4 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention is made clearly and completely with reference to the accompanying drawings.
Example 1
The method for detecting Cr in the solid agricultural product sample based on the ionic liquid aqueous two-phase comprises the following steps:
step one: weighing TBAH and EDTA, mixing and stirring for 30min in an aqueous solution according to the proportion of TBAH to EDTA to water=3.55 to 1:50, and then drying the solution to constant weight in a rotary evaporator to prepare the novel chelating phase-splitting agent EDTA-TBA;
step two: weighing 2g of mushroom sample powder, putting the powder into a dry small glass bottle, adding 5g of EDTA-TBA, adding pure water and 40% TBAH aqueous solution, dissolving in water bath at 30 ℃ and stirring for 2 hours, and standing at room temperature for 30min to enable the powder to be stable and phase-separated to be an upper phase and a lower phase;
step three: taking a lower phase solution, adjusting the pH value to be 2-3, completely precipitating chelating phase-splitting agent EDTA-TBA, filtering, taking the filtered solution, placing the filtered solution into a colorimetric tube, adding 1.5mL of 100g/L potassium persulfate solution, fully reacting, adding 4.5mL of 1mol/L sulfuric acid solution and 0.5mL of phosphoric acid (1:1, V/V), and shaking uniformly;
step four: 2.0mL of 2.5g/L diphenylcarbodihydrazide solution was added, the volume was fixed to 50mL with pure water, the mixture was shaken well, and the mixture was developed at room temperature for 10min. Three parallel experiments were performed with reagent blanks as reference, and absorbance was measured at 540nm by uv spectrophotometry using a 3cm cuvette.
Meanwhile, the traditional atomic absorption method is used for testing, the measured values are used as true values for comparison, the results are basically consistent, and the detection precision results are shown in table 1.
Example 2
The method for detecting Cr in the solid agricultural product sample based on the ionic liquid aqueous two-phase comprises the following steps:
step one: weighing TBAH and EDTA, mixing and stirring for 30min in an aqueous solution according to the proportion of TBAH to EDTA to water=3.55 to 1:50, and then drying the solution to constant weight in a rotary evaporator to prepare the novel chelating phase-splitting agent EDTA-TBA;
step two: weighing 2g of tea sample powder, putting into a dry small glass bottle, adding EDTA-TBA, adding pure water and 40% TBAH aqueous solution, heating in water bath at 20deg.C for dissolving, stirring for 4h, and standing at room temperature for 40min to stabilize phase separation;
step three: and taking out the phase solution, adjusting the pH to 2-3, completely precipitating the chelating phase-splitting agent EDTA-TBA, and filtering. Placing the filtered filtrate into a colorimetric tube, adding 1.5mL of 100g/L potassium persulfate solution, fully reacting, adding 4.5mL of 1mol/L sulfuric acid solution and 0.5mL of phosphoric acid (1:1, V/V), and shaking uniformly;
step four: 2.0mL of 2.5g/L diphenylcarbodihydrazide solution was added, the volume was fixed to 50mL with pure water, the mixture was shaken well, and the mixture was developed at room temperature for 10min. Three parallel experiments were performed with reagent blanks as reference. Absorbance was measured at 540nm by uv spectrophotometry using a 3cm cuvette;
meanwhile, the traditional atomic absorption method is used for testing, the measured values are used as true values for comparison, the results are basically consistent, and the detection precision results are shown in table 1.
Example 3
The dry tea sample powder from example 2 was replaced with a millet sample, the rest of the procedure remaining unchanged.
Meanwhile, the traditional atomic absorption method is used for testing, the measured values are used as true values for comparison, the results are basically consistent, and the detection precision results are shown in table 1.
Example 4
In order to optimize the oxidizing time of the oxidant in the third step of the invention, an optimization experiment is carried out, the absorbance of ultraviolet is taken as an optimization standard, namely the highest absorbance is the optimal, and the optimization result is shown in figure 1. The oxidant is selected from potassium persulfate and hydrogen peroxide, and the reaction time of the potassium persulfate is shorter than that of the hydrogen peroxide and the influence on absorbance is smaller than that of the hydrogen peroxide through experiments, so that the potassium persulfate is selected as the oxidant, and the temperature is raised for 20min at 80 ℃ to be suitable for the reaction.
While the basic principles, principal features and advantages of the present invention have been shown and described, it will be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are described in the foregoing description merely illustrate the principles of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined in the appended claims and their equivalents.
Claims (6)
1. The method for detecting Cr in the solid agricultural product sample based on the ionic liquid double water phase is characterized by comprising the following steps of: the method comprises the following steps:
step one, preparing a chelating phase-splitting agent;
weighing 2g of sample powder, putting the sample powder into a dry glass bottle, adding a chelating phase-splitting agent, adding pure water and 40% of ionic liquid aqueous solution, heating in a water bath at 20-30 ℃ to dissolve the sample powder, stirring the sample powder for 2-4 hours, standing the sample powder at room temperature for 30-40 min to enable the sample powder to be stable in phase separation, and separating the sample powder into an upper phase and a lower phase;
step three, taking down the phase solution, adjusting the pH value to be 2-3, completely precipitating the chelating phase-splitting agent, filtering, taking the filtered solution, placing the filtered solution into a colorimetric tube, adding the oxidant solution, fully reacting, adding 4.5mL of 1mol/L sulfuric acid solution and 0.5mL of phosphoric acid, and shaking uniformly to obtain the chelating phase-splitting agent;
and step four, adding 2.0mL of 2.5g/L diphenyl carbodihydrazide solution, fixing the volume to 50mL by using pure water, shaking uniformly, standing for 10min at room temperature, taking a reagent blank as a reference, performing three groups of parallel experiments for comparison, and measuring the absorbance at 540nm by using a 3cm cuvette through an ultraviolet spectrophotometry.
2. The method for detecting Cr in a solid agricultural product sample based on an ionic liquid aqueous two phase according to claim 1, wherein: the chelating phase-splitting agent in the first step is EDTA-TBA, and the preparation method comprises the following steps: TBAH and EDTA are weighed and in aqueous solution according to TBAH: EDTA: water = 3.55: 1:50, stirring for 30min, and drying the solution in a rotary evaporator to constant weight to obtain the chelating phase-splitting agent.
3. The method for detecting Cr in a solid agricultural product sample based on an ionic liquid aqueous two phase according to claim 1, wherein: in the second step, the ionic liquid is at least one of tetrabutylammonium hydroxide, tetrabutylammonium chloride, tetrabutylammonium bromide, 1- (2-naphthylmethyl) -3-methylimidazole acetate, 1-heptyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate, 1-benzyl-3-methylimidazole acetate, 1- (cyclohexylmethyl) -3-methylimidazole acetate and 1-butyl-3-methylimidazole chloride.
4. A method for detecting Cr in a solid agricultural product sample based on an ionic liquid aqueous two phase according to claim 1 or 3, characterized in that: in the second step, the ionic liquid is tetrabutylammonium hydroxide.
5. The method for detecting Cr in a solid agricultural product sample based on an ionic liquid aqueous two phase according to claim 1, wherein: in the phase separation in the second step, the dissolved solid agricultural product sample is kept in the upper phase, and Cr is separated into the lower phase.
6. The method for detecting Cr in a solid agricultural product sample based on an ionic liquid aqueous two phase according to claim 1, wherein: the oxidant solution in step three was 1.5mL 100g/L potassium persulfate solution.
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