CN103499537A - Method for determining content of zinc in mung beans by using cloud point extraction-atomic spectrum method - Google Patents
Method for determining content of zinc in mung beans by using cloud point extraction-atomic spectrum method Download PDFInfo
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Abstract
The invention provides a method for determining the content of zinc in mung beans by using a cloud point extraction-atomic spectrum method. The method is characterized by being comprising the flowing steps: pretreating mung bean samples by cold digestion and heating digestion through long-time soaking, combining 1-(2-pyridine azo)-2 naphthol (PAN) ethanol solution as a complexing agent with zinc to form a stable hydrophobic ionic associate after digestion, adding alkylphenol and ethylene oxide condensation compound to obtain a non-ionic surface active agent, extracting to obtain the non-ionic surface active agent organic phase, and determining the content of the zinc in the non-ionic surface active agent organic phase by using a flame atomic absorption spectrometry after dissolving and diluting of nitric acid and ethanol. The method solves the problems that a traditional method has low sensitivity to microelements and can be easily interfered by co-existing ions by using the flame atomic absorption spectrometry, and has the advantages of accuracy, reliability, high recovery rate, low relative standard deviation, high enrichment coefficient, rapidness and convenience.
Description
Technical field
The present invention relates to a kind of method of measuring zinc content in mung bean, be specifically related to the method for zinc content in a kind of mung bean of the Flame Atomic Absorption Spectrometry Determination by the cloud point extraction enrichment.
Background technology
The calorie value of mung bean is high, is rich in the various trace elements such as protein, phosphatide, dietary fiber, carbohydrates, vitamin E and phosphorus, calcium, iron, potassium, magnesium, manganese, zinc, copper, has high nutrition and health care and medical value.Wherein the zinc element in human body, participate in directly adjust and protein synthetic, and the merisis of cell and regeneration, also participate in the composition of liver and retina vitamin A reductase, the enzyme that contains the enzyme of zinc in human body and activated by zinc is up to kind more than 70, the appropriate absorption zinc of human body can enhance metabolism, and improves immunity.
Mung bean is top grade in the summertime diet, and the content of measuring zinc in mung bean can provide the reference data of use to the dietotherapy health-care efficacy, have certain practical value.Current modal analysis means mainly contains atomic absorption spectrophotometry, flow injection light scattering method, GFAAS (graphite furnace atomic absorption spectrometry), flame atomic absorption spectrometry, and wherein flame atomic absorption spectrometry is because its rapid and convenient, accuracy are high, favorable repeatability becomes one of common method of trace element determination and analysis.But in the mung bean sample, the content of zinc is lower, the absorption spectroscopy based on conventional comes the measurement result always can not be satisfactory, and be in particular in: sensitivity and accuracy are all lower, and coexisting ion disturbs large.
Summary of the invention
In order to solve the deficiency in background technology, the object of the invention is to overcome the defect of background technology, provide a kind of sensitivity, precision high, the cloud point extraction that not disturbed by coexisting ion-atomic spectroscopy is measured the method for zinc content in mung bean.
For achieving the above object, the technical solution used in the present invention is: a kind of cloud point extraction-atomic spectroscopy is measured the method for zinc content in mung bean, it is characterized in that: comprise the following steps:
A. sample collection: commercially available mung bean is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature roaster of 80 ℃, dry 6h, take out to be placed in and grind alms bowl and pulverize powdered, obtain the mung bean sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. Specimen eliminating is processed and is obtained sample solution: accurately take the mung bean sample in conical flask, after adding a small amount of water-wet, add again and clear up solvent, the described solvent of clearing up is that volume ratio is (4.5～5.5): 1 nitric acid, the perchloric acid mixed solution, soak that 30min is backward adds the beaded glass that diameter is 0.5mm again, cover the cold digestion of funnel, cold digestion is placed on heating and decompose on electric hot plate by conical flask after finishing, until test solution is limpid colourless and with white cigarette, and the volume that is evaporated to test solution is to clear up 1/4th of solvent adding amount volume, after test solution is cooled to room temperature, filtration obtains filtrate and is placed in volumetric flask, obtain sample solution with redistilled water dilution constant volume stand-by,
C. sample cloud point extraction separation and concentration is processed and obtained testing sample solution: the sample solution quantitatively obtained in removing step b is in centrifuge tube, splash into two dimethyl diaminophenazine chloride indicator solutions, extremely yellow with color toner solution, add complexing agent and sample solution to be thoroughly mixed to form the hydrophobicity ionic associate, shake up the standing rear pH to 5.0 that regulates mixed solution with buffer solution, then add 10% condensation compound of alkyl phenol and epoxy ethane solution, obtain the non-ionic surfactant micelle solution, then add the sodium chloride solution of 1.0mL2.0mmol/L to reduce cloud point temperature to 60～65 ℃, with after redistilled water dilution constant volume, shake up and be placed in 70～90 ℃ of water-baths and heat 2h, centrifugal 8min(3800r/min while hot) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, in lower floor's organic phase, add the nital of 0.1mol/L to be settled to 1mL, obtain testing sample solution,
D. the hydrochloric acid of 0.1mol/L of take is thinning agent, the zinc titer is mixed with to the series standard solution of variable concentrations, and measures the absorbance of series standard solution, sets up regression equation or drawing curve;
E. measure the absorbance of testing sample solution, according to the content of nickel in regression equation or drawing curve calculation testing sample solution;
F. cadmium content in the Instrument measuring rice sample: described instrument comprises: flame atomic absorption spectrophotometer, zinc hollow cathode lamp, and design parameter arranges as follows:
Analytical wavelengths: 283.3nm
Lamp current: 10mA
Spectral band-width: 0.4nm
Burner height: 10mm
Acetylene gas flow: 2.3L/min
Air mass flow: air mass flow: 9.5mL/min
In a preferred embodiment of the present invention, the volume that further comprises complexing agent addition described in step c is 40% of the sample solution amount of pipetting volume.
In a preferred embodiment of the present invention, further comprise in step c the 1-(2-pyridylazo that the described complexing agent that adds is 2.0mmol/L)-2 naphthols (PAN) ethanolic solutions.
In a preferred embodiment of the present invention, further comprise in step c that for the damping fluid of regulating mixed solution pH be the pH borax-boric acid mixed liquor that is 9.5.
In a preferred embodiment of the present invention, further comprise described in step b that clearing up solvent is nitric acid, the perchloric acid mixed solution that volume ratio is 4:1.
In a preferred embodiment of the present invention, further comprise that the time of cold digestion in step b is no less than 6h.
In a preferred embodiment of the present invention, further comprise that toner described in step c is the volume ratio ammoniacal liquor that is 9:1, the ammonia spirit of redistilled water.
In a preferred embodiment of the present invention, further comprise that in step b, the mung bean sample is 1:10 with the mass volume ratio g/mL that clears up solvent.
Usefulness of the present invention is: 1, cloud point extraction of the present invention-atomic spectroscopy is measured the method for zinc content in mung bean, the condensation compound of alkyl phenol and epoxy ethane (OP extractant) of take is surfactant, the 1-(2-pyridylazo)-2 to be complexing agent carry out the cloud point extraction enrichment to the sample solution of clearing up after processing to naphthols (PAN) ethanolic solution, improves sensitivity and the accuracy of analytical approach;
2,, by cloud point extraction and flame atomic absorption spectrometry combination, overcome the interference of coexisting ion to measuring in the matrix component, thereby improved the analytical performance of analytical approach;
3, in the extracting and enriching process, add the sodium chloride solution of 2.0mmol/L to reduce cloud point temperature, be beneficial to the carrying out of phase-splitting operation, improve the absorbance of zinc;
4, clear up in processing procedure after clearing up solvent soaking and add beaded glass, guarantee that Sample Dilution is abundant, thereby improve the accuracy of experimental result.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is further detailed explanation.
The present invention proposes following cloud point extraction-atomic spectroscopy (FAAS method) and measure the method for zinc content in mung bean:
1, equipment and reagent
(1) AA6800 flame atomic absorption spectrophotometer (attached computing machine and printer);
(2) zinc hollow cathode lamp;
(3) pH-3C type acidometer;
(4) electronic analytical balance, precision 0.0001mg;
(5) 80-1 type low speed centrifuge and HH-4 digital display thermostat water bath
(6) temperature controlled water bath pot, electric hot plate
(7) borax-borate buffer solution that pH is 9.5; 2.0mmol/L sodium chloride solution; 2.0mmol/L the PAN ethanolic solution; 10% condensation compound of alkyl phenol and epoxy ethane solution; 0.1mol/L nital; (1+1) salpeter solution; (1+1) perchloric acid solution;
(8) preparation of zinc series standard solution: get respectively different volumes, concentration is the Zinc standard solution of 1ug/mL in volumetric flask, with hydrochloric acid, dilutes constant volume, shakes up.Obtain as required the series standard solution of 0～0.8ug/mL during use with the hydrochloric acid stepwise dilution.
2, the atomic absorption spectrometry condition is as follows:
Analytical wavelengths: 283.3nm
Lamp current: 10mA
Spectral band-width: 0.4nm
Burner height: 10mm
Acetylene gas flow: 2.3L/min
Air mass flow: air mass flow: 9.5mL/min
3, determination and analysis method
(1) sample collection:
Commercially available mung bean is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature roaster of 80 ℃, dry 6h, take out to be placed in and grind alms bowl and pulverize powdered, obtain the mung bean sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
(2) Specimen eliminating is processed and is obtained sample solution:
Accurately take the mung bean sample in conical flask, after adding a small amount of water-wet, add again and clear up solvent, wherein clearing up solvent is that volume ratio is (4.5～5.5): 1 nitric acid, perchloric acid mixed solution, preferred volume ratio is 4:1, digestion is complete, and mung bean sample herein is 1:10 with the mass volume ratio g/mL that clears up solvent; Soak that 30min is backward adds the beaded glass that diameter is 0.5mm again, cover the cold digestion of funnel, the time of cold digestion herein is no less than 6h, cold digestion is placed on heating and decompose on electric hot plate by conical flask after finishing, until test solution is limpid colourless and with white cigarette, and the volume that is evaporated to test solution is to clear up 1/4th of solvent adding amount volume, filter after test solution is cooled to room temperature and obtain filtrate and be placed in volumetric flask, obtain sample solution with redistilled water dilution constant volume stand-by;
(3) sample cloud point extraction separation and concentration is processed and is obtained testing sample solution:
The sample solution quantitatively obtained in removing step b is in centrifuge tube, splash into two dimethyl diaminophenazine chloride indicator solutions, extremely yellow with color toner solution, toner herein is the volume ratio ammoniacal liquor that is 9:1, the ammonia spirit of redistilled water, add complexing agent and sample solution to be thoroughly mixed to form the hydrophobicity ionic associate, the 1-(2-pyridylazo that complexing agent herein is 2.0mmol/L)-2 naphthols (PAN) ethanolic solutions, and the volume of complexing agent addition is 40% of the sample solution amount of pipetting volume, shake up the standing rear pH to 5.0 that regulates mixed solution with buffer solution, damping fluid herein is the pH borax-boric acid mixed liquor that is 9.5, then add 10% condensation compound of alkyl phenol and epoxy ethane solution, obtain the non-ionic surfactant micelle solution, then add the sodium chloride solution of 1.0mL2.0mmol/L to reduce cloud point temperature to 50～65 ℃, with after redistilled water dilution constant volume, shake up and be placed in 70～90 ℃ of water-baths and heat 2h, centrifugal 8min(3800r/min while hot) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, in lower floor's organic phase, add the nital of 0.1mol/L to be settled to 1mL, obtain testing sample solution,
(4) preparation series standard solution drawing curve:
The Zinc standard solution that pipette respectively 0.0,1.0,2.0,4.0,6.0,8.0mL is 1ug/mL in concentration is in the 10mL volumetric flask, with the hydrochloric acid of 0.1mol/L, it is thinning agent, the dilution constant volume, obtain being respectively containing zinc concentration A the series standard solution of 0ug/mL, 0.1ug/mL, 0.2ug/mL, 0.4ug/mL, 0.6ug/mL, 0.8ug/mL, then measure the absorbance C of series standard solution according to above-mentioned atomic absorption spectrometry condition, as follows: C=-0.0211,0.3573,0.7358,1.4928,2.2498,3.0068.
According to the corresponding relation of A and C, obtain an equation of linear regression by Mathematical Fitting, as follows:
A=0.2462C(ug/mL)+0.0056, related coefficient is r=0.9995.
Embodiment 1:
Specimen eliminating is processed and is obtained sample solution:
Accurately take 1g mung bean sample and be placed in clean dry 150mL conical flask, after adding a small amount of water-wet, then add and clear up solvent and soak, wherein clear up the nitric acid of solvent 8mL and the perchloric acid mixed solution of 2mL, prepare blank solution simultaneously; Soak that 30min is backward adds the beaded glass that several diameters are 0.5mm again, then after covering funnel, cold digestion is no less than 6h, cold digestion is placed on heating and decompose on electric hot plate by conical flask after finishing, until test solution is limpid colourless and with white cigarette, and to be evaporated to residue test solution volume be 2mL, after test solution is cooled to room temperature, filtration obtains filtrate and is placed in the 25mL volumetric flask, obtains sample solution with redistilled water dilution constant volume stand-by.
Sample cloud point extraction separation and concentration is processed and is obtained testing sample solution:
Quantitatively pipette the 2.5mL sample solution in the 10mL centrifuge tube, splash into two dimethyl diaminophenazine chloride indicator solutions, extremely yellow with the ammoniacal liquor toning solution of 9:1, the 1-(2-pyridylazo that adds 1.0mL2.0mmol/L)-2 naphthols (PAN) ethanolic solutions are as complexing agent, make complexing agent and sample solution be thoroughly mixed to form the lyophobic association thing, shake up after standing the pH to 5.0 that adds the borax that 1mLpH is 9.5-boric acid mixed liquor to regulate mixed solution, then the condensation compound of alkyl phenol and epoxy ethane solution that adds 0.5mL10%, obtain the non-ionic surfactant micelle solution, then add the sodium chloride solution of 1.0mL2.0mmol/L to reduce cloud point temperature to 50～65 ℃, with after redistilled water dilution constant volume, shake up and be placed in 85 ℃ of water-baths and heat 2h, centrifugal 8min(3800r/min while hot) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, in lower floor's organic phase, add the nital of 0.1mol/L to be settled to 1mL, obtain testing sample solution,
The mensuration of sample absorbance:
Carry out the mensuration of testing sample solution absorbance under above-mentioned same parameters arranges, prepare 6 parts of parallel testing sample solutions, calculate respectively the content of cadmium element in this 6 duplicate samples according to equation of linear regression, average.The nickel element content recorded is respectively: 30.81mg/Kg, 31.45mg/Kg, 32.09mg/Kg, 29.98mg/Kg, 30.73mg/Kg, 31.67mg/Kg, calculating mean value is 31.12mg/Kg.
Recovery experiment:
For recovery experiment has been carried out in method of inspection accuracy, in the actual sample analytic process, this step is omitted.
Pipette respectively testing sample solution 5.0mL sample liquid in conical flask, then the Zinc standard solution 1mL that adds respectively three kinds of variable concentrations in each conical flask, measured by experimental technique of the present invention, do blank and recovery testu simultaneously, result is as following table 1-1:
Table 1-1
| The concentration numbering | Add scalar/(mg.Kg -1） | Measured value/(mg.Kg -1） | The recovery/% |
| 1 | 10 | 10.2 | 102 |
| 2 | 15 | 14.2 | 94.7 |
| 3 | 20 | 19.6 | 98 |
Can find out that by table 1-1 with the recovery of standard addition of zinc content in method mensuration mung bean of the present invention be between 94.7～102%, calculating relative standard deviation is 2.5%, highly sensitive, accurate, quick.
Coexisting ion impact experiment:
Carried out coexisting ion impact experiment for the anti-interference of the method for inspection, in the actual sample analytic process, this step is omitted.
Adding between complexing agent to the interfering ion that adds inhomogeneity, different amounts in the 0.5ug/mL Zinc standard solution, then according to its absorbance of determination of experimental method, calculate recovery rate, if the recovery is 90～110% the time, be referred to as the mensuration of zinc is not brought to interference, record result as following table 1-2
Table 1-2
| Coexisting ion | Coexisting ion/zinc (W/W) | The recovery (%) |
| Cu 2+ | 500 | 107 |
| Mn 2+ | 50 | 93 |
| Fe 2+ | 2 | 92 |
| Fe 3+ | 2 | 93 |
| Ca 2+ | 200 | 109 |
| Mg 2+ | 100 | 98 |
| K + | 80 | 109 |
By table, 1-1 can find out, in the inventive method, the mensuration of zinc content is not subject to the interference of coexisting ion.
Embodiment 2:
With the difference of embodiment 1, only be: in sample cloud point extraction preenrichment processing procedure, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 70 ℃ of water-baths and heat 2h.
Other experiment condition is consistent with embodiment 1, and experimental result shows, when bath temperature is 70 ℃, the cloud point phenomenon does not appear in solution, and the cloud point extraction experiment can't be carried out.
Embodiment 3:
With the difference of embodiment 1, only be: in sample cloud point extraction preenrichment processing procedure, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 75 ℃ of water-baths and heat 2h.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of zinc element in this 6 duplicate samples according to equation of linear regression, averages.The zinc constituent content recorded is respectively: 28.42mg/Kg, 29.35mg/Kg, 29.87mg/Kg, 28.68mg/Kg, 29.03mg/Kg, 29.46mg/Kg, calculating mean value is 29.15mg/Kg.With respect to embodiment 1 and embodiment 2, draw, bath temperature has the cloud point phenomenon to produce in the time of 75 ℃, and the absorbance recorded has the trend of increase with the rising of temperature.
Embodiment 4:
With the difference of embodiment 1, only be: in sample cloud point extraction preenrichment processing procedure, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 90 ℃ of water-baths and heat 2h.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of zinc element in this 6 duplicate samples according to equation of linear regression, averages.The zinc constituent content recorded is respectively: 29.82mg/Kg, 30.91mg/Kg, 31.32mg/Kg, 29.03mg/Kg, 30.23mg/Kg, 30.76mg/Kg, calculating mean value is: 30.35mg/Kg.With respect to embodiment 1 absorbance that can to find out at bath temperature be zinc under 90 ℃ of conditions, in stable, descend to some extent.
Therefore, in quantitative test of the present invention, best bath temperature is 85 ℃.
Embodiment 5:
With the difference of embodiment 1, only be: directly carry out examination with computer after clearing up processing, do not have the cloud point extraction preenrichment to process.
Other experiment condition is consistent, prepares 6 parts of parallel sample solutions, calculates respectively the content of zinc element in this 6 duplicate samples according to equation of linear regression, averages.The zinc constituent content recorded is respectively: 19.38mg/Kg, 20.12mg/Kg, 19.46mg/Kg, 18.95mg/Kg, 19.53mg/Kg, 20.26mg/Kg, calculating mean value is: 19.62mg/Kg.
Recovery experiment:
For recovery experiment has been carried out in method of inspection accuracy, in the actual sample analytic process, this step is omitted.
Pipette respectively testing sample solution 5.0mL sample liquid in conical flask, then the Zinc standard solution 1mL that adds respectively three kinds of variable concentrations in each conical flask, measured by experimental technique of the present invention, do blank and recovery testu simultaneously, result is as following table 2-1:
Table 2-1
| The concentration numbering | Add scalar/(mg.Kg -1） | Measured value/(mg.Kg -1） | The recovery/% |
| 1 | 10 | 8.2 | 82 |
| 2 | 15 | 13.1 | 87.3 |
| 3 | 20 | 17.3 | 86.5 |
Can be found out with the recovery of standard addition of zinc content in the method mensuration mung bean of embodiment 5 by table 2-1 and be
Between 82～87.3%, calculating relative standard deviation is 3.1%.
Coexisting ion impact experiment:
Carried out coexisting ion impact experiment for the anti-interference of the method for inspection, in the actual sample analytic process, this step is omitted.
Adding between complexing agent to the interfering ion that adds inhomogeneity, different amounts in the 0.5ug/mL Zinc standard solution, then according to its absorbance of determination of experimental method, calculate recovery rate, if the recovery is 90～110% the time, be referred to as the mensuration of zinc is not brought to interference, record result as following table 2-2
Table 2-2
| Coexisting ion | Coexisting ion/zinc (W/W) | The recovery (%) |
| Cu 2+ | 356 | 86 |
| Mn 2+ | 43 | 78 |
| Fe 2+ | 1.2 | 75 |
| Fe 3+ | 1.2 | 76 |
| Ca 2+ | 168 | 81 |
| Mg 2+ | 82 | 79 |
| K + | 68 | 87 |
With respect to embodiment 1, recovery variation, coexisting ion disturb strong, therefore, with experimental technique of the present invention, come zinc content in the quantitative test mung bean to improve sensitivity and antijamming capability.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify and all should be equivalent substitute mode, within being included in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (8)
1. a cloud point extraction-atomic spectroscopy is measured the method for zinc content in mung bean, it is characterized in that: comprise the following steps:
A. sample collection: commercially available mung bean is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature roaster of 80 ℃, dry 6h, take out to be placed in and grind alms bowl and pulverize powdered, obtain the mung bean sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. Specimen eliminating is processed and is obtained sample solution: accurately take the mung bean sample in conical flask, after adding a small amount of water-wet, add again and clear up solvent, the described solvent of clearing up is that volume ratio is (4.5 ~ 5.5): 1 nitric acid, the perchloric acid mixed solution, soak that 30min is backward adds the beaded glass that diameter is 0.5mm again, cover the cold digestion of funnel, cold digestion is placed on heating and decompose on electric hot plate by conical flask after finishing, until test solution is limpid colourless and with white cigarette, and the volume that is evaporated to test solution is to clear up 1/4th of solvent adding amount volume, after test solution is cooled to room temperature, filtration obtains filtrate and is placed in volumetric flask, obtain sample solution with redistilled water dilution constant volume stand-by,
C. sample cloud point extraction separation and concentration is processed and obtained testing sample solution: the sample solution quantitatively obtained in removing step b is in centrifuge tube, splash into two dimethyl diaminophenazine chloride indicator solutions, extremely yellow with color toner solution, add complexing agent and sample solution to be thoroughly mixed to form the hydrophobicity ionic associate, shake up the standing rear pH to 5.0 that regulates mixed solution with buffer solution, then add 10% condensation compound of alkyl phenol and epoxy ethane solution, obtain the non-ionic surfactant micelle solution, then add the sodium chloride solution of 1.0mL 2.0mmol/L to reduce cloud point temperature to 60 ~ 65 ℃, with after redistilled water dilution constant volume, shake up and be placed in 70 ~ 90 ℃ of water-baths and heat 2h, centrifugal 8min(3800r/min while hot) make its phase-splitting, be cooled to zero degree after the solution phase-splitting in ice bath, remove the upper strata water, in lower floor's organic phase, add the nital of 0.1mol/L to be settled to 1mL, obtain testing sample solution,
D. the hydrochloric acid of 0.1mol/L of take is thinning agent, the zinc titer is mixed with to the series standard solution of variable concentrations, and measures the absorbance of series standard solution, sets up regression equation or drawing curve;
E. measure the absorbance of testing sample solution, according to the content of nickel in regression equation or working curve calculating testing sample solution;
F. cadmium content in the Instrument measuring rice sample: described instrument comprises: flame atomic absorption spectrophotometer, zinc hollow cathode lamp, and design parameter arranges as follows:
Analytical wavelengths: 283.3nm
Lamp current: 10mA
Spectral band-width: 0.4nm
Burner height: 10mm
Acetylene gas flow: 2.3 L/min
Air mass flow: air mass flow: 9.5mL/min.
2. cloud point extraction according to claim 1-atomic spectroscopy is measured the method for zinc content in mung bean, and it is characterized in that: the volume of the addition of complexing agent described in step c is 40% of the sample solution amount of pipetting volume.
3. cloud point extraction according to claim 2-atomic spectroscopy is measured the method for zinc content in mung bean, it is characterized in that: the 1-(2-pyridylazo that the described complexing agent added in step c is 2.0mmol/L)-2 naphthols (PAN) ethanolic solutions.
4. cloud point extraction according to claim 1-atomic spectroscopy is measured the method for zinc content in mung bean, it is characterized in that: in step c, for the damping fluid of regulating mixed solution pH, be the pH borax-boric acid mixed liquor that is 9.5.
5. cloud point extraction according to claim 1-atomic spectroscopy is measured the method for zinc content in mung bean, and it is characterized in that: clearing up solvent described in step b is nitric acid, the perchloric acid mixed solution that volume ratio is 4:1.
6. cloud point extraction according to claim 1-atomic spectroscopy is measured the method for zinc content in mung bean, and it is characterized in that: in step b, the time of cold digestion is no less than 6h.
7. cloud point extraction according to claim 1-atomic spectroscopy is measured the method for zinc content in mung bean, it is characterized in that: toner described in step c is the volume ratio ammoniacal liquor that is 9:1, the ammonia spirit of redistilled water.
8. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 1 is characterized in that: in step b, the mung bean sample is 1:10 with the mass volume ratio g/mL that clears up solvent.
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| CN107870155A (en) * | 2017-11-15 | 2018-04-03 | 云南省农业科学院甘蔗研究所 | The detection method of Zn content in a kind of sugarcane sugarcane juice |
| CN109164052A (en) * | 2018-10-09 | 2019-01-08 | 江苏农牧科技职业学院 | A kind of extraction element of Chinese herbaceous peony scape Mineral Elements Content |
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