CN103499549A - Method for measuring content of trace cadmium in rice by utilizing flame atomic absorption spectrometry - Google Patents
Method for measuring content of trace cadmium in rice by utilizing flame atomic absorption spectrometry Download PDFInfo
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Abstract
The invention provides a method for measuring the content of trace cadmium in rice by utilizing a flame atomic absorption spectrometry. The method is characterized by comprising the following steps of preprocessing a rice sample by utilizing a microwave digestion manner in which a long-time soaking manner is combined with a step type heating manner, after the digestion, reacting cadmium ions with potassium iodide to generate CdI4<2->, reacting the CdI4<2-> with methyl green (MG) to generate a hydrophobic ionic association compound, extracting the hydrophobic ionic association compound into a micelle phase of a TritonX-114 nonionic surfactant, and measuring the cadmium content in the micelle phase by utilizing the flame atomic absorption spectrometry. The method solves the problems that the measurement of the trace cadmium by utilizing a traditional flame atomic absorption spectrometry is low in sensitivity and is easily interfered by matrixes and has the advantages of high precision and recovery rate, small relative standard deviation, accuracy, reliability, rapidness and convenience.
Description
Technical field
The present invention relates to measure the method for trace amount of cadmium in rice, be specifically related to the method for trace amount of cadmium in a kind of rice of the Flame Atomic Absorption Spectrometry Determination by micro-wave digestion-cloud point extraction.
Background technology
Every being a kind of toxic metals element with strongly carcinogenic and teratogenesis; after the absorption inside of human body is absorbed; discharge very slow; be about 16～38 years in the human-body biological half life period; cadmium is accumulated in the kidney of human body and liver; cause accumulation property poisoning, can make skeleton pain, fracture, even cause cancer.In recent years due to the factor of environment, quite a few cadmium is by grain and vegetables, for example, rice, flour etc. enter human body, the cadmium of wherein taking in grain accounts for half of total intake, more and more be subject to the common concern of the world today containing the cadmium problem in grain, therefore, necessary sensitive, the determination and analysis method accurately of setting up trace amount of cadmium in grain.
Current modal trace element analysis means mainly contain 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 analyzing the matrix complex sample during trace element, the sensitivity that it is lower and matrix disturb and have greatly limited its range of application, and therefore, task of the present invention just is to provide a kind of assay method that can improve the sensitivity of Flame Atomic Absorption Spectrometry Determination Determination of Trace Amount Cadmium and antijamming capability.
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, the method for trace amount of cadmium in a kind of highly sensitive, Flame Atomic Absorption Spectrometry Determination rice that can improve anti-matrix interference performance is provided.
For achieving the above object, the technical solution used in the present invention is: a kind of method of trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice is characterized in that: comprise the following steps:
A. sample collection: commercially available rice is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature oven of 100 ℃, dry 2h, take out to be placed in and grind alms bowl and pulverize powdered, obtain rice sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. the sample micro-wave digestion is processed and is obtained sample solution: accurately take rice sample and be placed in clean dry teflon pressure dispelling tank, add and clear up solvent soaking and spend the night, the described solvent of clearing up is that massfraction is respectively 65% nitric acid 1mL, the mixed solvent of 30% hydrogen peroxide 3mL, prepare blank solution simultaneously, then seal and put into microwave digestion device according to micro-wave digestion program heating and decompose, after clearing up EOP (end of program), take out counteracting tank and be cooled to room temperature, shift sample to polytetrafluoroethylene beaker, beaker is placed in to low-temperature heat on electric hot plate and catches up with acid, until sample evaporation during to quick-drying, take off beaker cooling and shift test solution to volumetric flask, dilute constant volume with redistilled water, shake up and obtain sample solution, and under the environment of 6 ℃, preserve stand-by,
C. the preenrichment of sample cloud point extraction is processed and obtained testing sample solution: the sample solution quantitatively obtained in removing step b is in centrifuge tube, add the fully mixed hydrophobicity ionic associate that forms of complexing agent and sample solution, shake up the standing rear pH to 4.0 with damping fluid adjusting mixed solution～5.0, then add 4.5% Triton-114 solution, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 40～60 ℃ of water-baths and be heated to cloud point temperature, centrifugal 10min(3800r/min while hot) make its phase-splitting, after the solution phase-splitting, ice bath is cooled to room temperature, remove the upper strata water, to the nital that adds 0.1mol/L in the rich micellar phase of lower floor, obtain testing sample solution,
D. standard solution preparation: take redistilled water as thinning agent, will be mixed with every titer the series standard solution of variable concentrations;
E. in the Instrument measuring rice sample every cadmium content: described instrument comprises: flame atomic absorption spectrophotometer, cadmium hollow cathode lamp, design parameter arranges as follows:
Analytical wavelengths: 228.8nm
Lamp current: 20mA
Spectral band-width: 0.4nm
Burner height: 5mm
Acetylene gas flow: 1.3L/min
Air mass flow: air mass flow: 8.0mL/min
F. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, the drawing standard curve, according to the content of nickel in typical curve or regression equation calculation testing sample solution.
In a preferred embodiment of the present invention, the volume that further comprises the addition of complexing agent described in step c is 40%～50% of the sample solution amount of pipetting volume.
In a preferred embodiment of the present invention, further comprise in step c the potpourri of the methyl green (MG) of potassium iodide that the described complexing agent added is the volume ratio 2mol/L that is 1:1 and 1.5mmol/L.
In a preferred embodiment of the present invention, the volume that further comprises the addition of Triton-114 solution in step c is 20%～30% of described complexing agent addition volume.
In a preferred embodiment of the present invention, further comprise that the program of clearing up of setting in microwave digestion device in step b is staged intensification heating and decompose program, be specially, 200 ℃ of heating 5min, 220 ℃ of heating 5min, 240 ℃ of heating 10min, 200 ℃ of heating 5min.
In a preferred embodiment of the present invention, further comprise that in step b, rice sample is 1:8.25 with the mass volume ratio g/mL that clears up solvent.
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 NaOH-potassium dihydrogen phosphate mixed liquor that is 4.0.
Usefulness of the present invention is: 1, the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice of the present invention, take Triton-114 as surfactant, the potpourri that volume ratio is 1:1 potassium iodide and methyl green is that the sample solution after complexing agent is processed micro-wave digestion carries out cloud point extraction, improve the atomization efficiency of cadmium atom in rice sample, improve measurement sensitivity;
2,, by cloud point extraction and flame atomic absorption spectrometry combination, overcome the interference of matrix component to measuring in the complex sample, thereby improved the analytical performance of analytical approach;
3, utilize the heating of microwave staged to assist and clear up, microwave energy directly penetrates sample inside, inside and outside heating simultaneously, and heating is fast, high, the molten sample that heats up is fast;
4, for fear of because reaction is too violent or decompose a large amount of gas produced, pressure being risen sharply, the present invention adopts staged intensification heating to make to clear up smoothly and completes.
5, rice sample is placed in and clears up the first soaked overnight of solvent, makes sample and clears up solvent and fully react, and can make nickel hard to tolerate fully clear up fast;
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 micro-wave digestion-cloud point extraction flame atomic absorption spectrometry (FAAS method) and measure the determination and analysis method of trace amount of cadmium in rice:
1, equipment and reagent
(1) AA6800 flame atomic absorption spectrophotometer (attached computing machine and printer);
(2) cadmium 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) MDS-8 microwave dissolver
(7) NaOH-potassium dihydrogen phosphate buffer solution that pH is 4.0; 2.0mol/L potassium iodide; 1.5mol/L methyl green; 4.5% TritonX-114 solution; 0.1mol/L the nitric acid methanol solution; (65%, 1+1) HNO
3; 30%H
2o
2;
(8) preparation of cadmium ion standard inventory solution and standard solution: accurately take 0.2152CdCl
2.25H
2o, in beaker, dissolves with redistilled water, is transferred to constant volume in the 100mL volumetric flask, shakes up.During use, use as required the redistilled water stepwise dilution to 0.5ng/mL～4ng/mL.
2, the atomic absorption spectrometry condition is as follows:
Analytical wavelengths: 228.8nm
Lamp current: 20mA
Spectral band-width: 0.4nm
Burner height: 5mm
Acetylene gas flow: 1.3L/min
Air mass flow: air mass flow: 8.0mL/min
3, determination and analysis method
(1) sample collection:
Commercially available rice is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature oven of 100 ℃, dry 2h, take out to be placed in and grind alms bowl and pulverize powdered, obtain rice sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
(2) the sample micro-wave digestion is processed and is obtained sample solution:
Accurately take rice sample and be placed in clean dry teflon pressure dispelling tank, add and clear up solvent soaking and spend the night, wherein clear up solvent and be the mixed solvent that massfraction is respectively 65% nitric acid 1mL, 30% hydrogen peroxide 3mL, rice sample is 1:8.25 with the mass volume ratio g/mL that clears up solvent herein, prepare blank solution simultaneously, then seal and put into microwave digestion device according to micro-wave digestion program heating and decompose, the heating and decompose program setting is that staged heats up, be specially, 200 ℃ of heating 5min, 220 ℃ of heating 5min, 240 ℃ of heating 10min, 200 ℃ of heating 5min, after clearing up EOP (end of program), take out counteracting tank and be cooled to room temperature, shift sample to the 50mL polytetrafluoroethylene beaker, beaker is placed in to low-temperature heat on electric hot plate and catches up with acid, until sample evaporation during to quick-drying, take off beaker cooling and shift test solution to the 25mL volumetric flask, dilute constant volume with redistilled water, shake up and obtain sample solution, and under the environment of 6 ℃, preserve stand-by,
(3) preenrichment of sample cloud point extraction is processed and is obtained testing sample solution:
Quantitatively pipette sample solution in centrifuge tube, add the fully mixed hydrophobicity ionic associate that forms of complexing agent and sample solution, the potpourri of the potassium iodide that complexing agent herein is the volume ratio 2mol/L that is 1:1 and the methyl green (MG) of 1.5mmol/L, and the volume of the addition of complexing agent is 40%～50% of the sample solution amount of pipetting volume; Shake up the standing rear pH to 4.0 with damping fluid adjusting mixed solution～5.0, buffer solution herein is the pH NaOH-potassium dihydrogen phosphate mixed liquor that is 4.0, then add 4.5% Triton-114 solution, obtain the non-ionic surfactant micelle solution, the volume of the addition of Triton-114 solution is 20%～30% of complexing agent addition volume herein; With redistilled water, it is diluted to constant volume, shake up to be placed in 40～60 ℃ of water-baths and be heated to cloud point temperature, centrifugal 10min(3800r/min while hot) make its phase-splitting, after the solution phase-splitting, ice bath is cooled to room temperature, remove the upper strata water, the nital to adding 0.1mol/L in the rich micellar phase of lower floor, obtain testing sample solution;
(4) preparation series standard solution drawing curve:
The cadmium standard solution that accurately pipette 0.0,0.25,0.50,1.00,1.50,2.00mL is 20ng/mL in concentration is in the 10mL volumetric flask, dilute constant volume with redistilled water, obtain being respectively containing cadmium concentration A the standard serial solution of 0ng/mL, 0.5ng/mL, 1.0ng/mL, 2.0ng/mL, 3.0ng/mL, 4.0ng/mL, then measure the absorbance C of series standard solution according to above-mentioned atomic absorption spectrometry condition, as follows: C=-0.049,4.902,6.618,19.828,29.778,39.728
According to the corresponding relation of A and C, obtain an equation of linear regression by Mathematical Fitting, as follows:
A=0.1005C(ng/mL)+0.0073, related coefficient is r=0.9998.
Embodiment 1:
The mensuration recovery of cadmium content experiment in the rice of northeast:
The sample micro-wave digestion is processed and is obtained sample solution:
Accurately take the 0.485g rice sample and be placed in clean dry 50mL teflon pressure dispelling tank, add and clear up solvent soaking and spend the night, wherein clearing up solvent is that massfraction is respectively 65% nitric acid 1mL, the mixed solvent of 30% hydrogen peroxide 3mL, prepare blank solution simultaneously, then seal and put into microwave digestion device according to micro-wave digestion program heating and decompose, the heating and decompose program setting is that staged heats up, be specially, 200 ℃ of heating 5min, 220 ℃ of heating 5min, 240 ℃ of heating 10min, 200 ℃ of heating 5min, after clearing up EOP (end of program), take out counteracting tank and be cooled to room temperature, shift sample to the 50mL polytetrafluoroethylene beaker, beaker is placed in to low-temperature heat on electric hot plate and catches up with acid, until sample evaporation during to quick-drying, take off beaker cooling and shift test solution to the 25mL volumetric flask, dilute constant volume with redistilled water, shake up and obtain sample solution, and under the environment of 6 ℃, preserve stand-by.
The preenrichment of sample cloud point extraction is processed and is obtained testing sample solution:
Quantitatively pipette the 9mL sample solution in the 15mL centrifuge tube, add the fully mixed hydrophobicity ionic associate that forms of complexing agent and sample solution, methyl green (MG) solution that adds successively potassium iodide and the 2mL1.5mmol/L of 2mL2mol/L, shake up after standing and add the damping fluid of NaOH-potassium dihydrogen phosphate that pH is 4.0 to the pH to 4.0 of mixed solution～5.0, then the Triton-114 solution that adds 1mL4.5%, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 50 ℃ of water-baths and be heated to cloud point temperature, centrifugal 10min(3800r/min while hot) make its phase-splitting, after the solution phase-splitting, ice bath is cooled to room temperature, remove the upper strata water, in the rich micellar phase of lower floor, add the nital of 0.1mol/L to be settled to 0.6mL.
The mensuration of sample absorbance:
Carry out the mensuration of testing sample solution 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 cadmium element content recorded is respectively: 50.7ug/Kg, 49.8ug/Kg, 52.3ug/Kg, 53.0ug/Kg, 51.4ug/Kg, 48.9ug/Kg, and calculating mean value is 51.02ug/Kg, content is up to standard.
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 counteracting tank, then the cadmium standard solution 1mL that adds respectively three kinds of variable concentrations in each counteracting tank, then carry out the mensuration of micro-wave digestion-cloud point extraction and absorbance with the same measured process, result is as following table 1:
Table 1
| The concentration numbering | Add scalar/(ug.g -1） | Measured value/(ug.g -1） | The recovery/% |
| 1 | 0.5 | 0.47 | 94 |
| 2 | 1.0 | 0.98 | 98 |
| 3 | 2.0 | 1.97 | 98.5 |
As can be seen from Table 1 in the rice of northeast cadmium content lower than rice cadmium maximum permissible concentration value in GB; Recovery of standard addition is between 94～98.5%, and calculating relative standard deviation is 1.6%, and it is sensitive, accurate, quick that visible the present invention measures in rice cadmium content.
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 40 ℃ of water-baths and be heated to cloud point temperature.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of cadmium element in this 6 duplicate samples according to equation of linear regression, averages.The cadmium element content recorded is respectively: 47.8ug/Kg, 46.9ug/Kg, 48.3ug/Kg, 49.2ug/Kg, 48.5ug/Kg, 46.3ug/Kg, calculating mean value is 47.83ug/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 counteracting tank, then the cadmium standard solution 1mL that adds respectively three kinds of variable concentrations in each counteracting tank, then in the same measured process, (bath temperature is 40 ℃) carries out the mensuration of micro-wave digestion-cloud point extraction and absorbance, and result is as following table 2:
Table 2
| The concentration numbering | Add scalar/(ug.g -1） | Measured value/(ug.g -1） | The recovery/% |
| 1 | 0.5 | 0.45 | 90 |
| 2 | 1.0 | 0.96 | 96 |
| 3 | 2.0 | 1.93 | 96.5 |
With respect to embodiment 1, in the rice recorded, the content of cadmium element is on the low side, then associative list 1 and table 2, can find out at bath temperature to be that under 40 ℃ of conditions, cadmium ion is not extracted fully, and absorbance is not maximum.
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 40 ℃ of water-baths and be heated to cloud point temperature.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel testing sample solutions, calculates respectively the content of cadmium element in this 6 duplicate samples according to equation of linear regression, averages.The cadmium element content recorded is respectively: 49.3ug/Kg, 48.3ug/Kg, 50.9ug/Kg, 51.8ug/Kg, 52.3ug/Kg, 49.2ug/Kg, calculating mean value is 50.30ug/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 counteracting tank, then the cadmium standard solution 1mL that adds respectively three kinds of variable concentrations in each counteracting tank, then in the same measured process, (bath temperature is 60 ℃) carries out the mensuration of micro-wave digestion-cloud point extraction and absorbance, and result is as following table 3:
Table 3
| The concentration numbering | Add scalar/(ug.g -1） | Measured value/(ug.g -1） | The recovery/% |
| 1 | 0.5 | 0.46 | 92 |
| 2 | 1.0 | 0.96 | 96 |
| 3 | 2.0 | 1.95 | 97.5 |
With respect to embodiment 1, in the rice recorded, the content of cadmium element is on the low side, then associative list 1 and table 2, the absorbance that can to find out at bath temperature be cadmium ion under 60 ℃ of conditions obviously descends, and analysis-by-synthesis draws, when bath temperature and equilibrium temperature are greater than 50 ℃, along with the rising of temperature, MG and CdI
4 2-weak interaction force between ion reduces, thereby reduces hydrophobicity ionic associate MG (CdI
4) stability, cause percentage extraction to reduce.
Therefore, in quantitative analysis method of the present invention, best bath temperature is 50 ℃.
Embodiment 4:
With the difference of embodiment 1, only be: micro-wave digestion directly carries out examination with computer after processing, and does 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 cadmium element in this 6 duplicate samples according to equation of linear regression, averages.The cadmium element content recorded is respectively: 45.3ug/Kg, 46.2ug/Kg, 45.8ug/Kg, 44.3ug/Kg, 45.9ug/Kg, 46.5ug/Kg, and calculating mean value is: 45.67ug/Kg; The rate that simultaneously is recycled is 90.5～93.2%, and the relative standard deviation of calculating is 3.0%.
With respect to embodiment 1, the equal variation of the recovery and relative standard deviation, therefore, the present invention adopts micro-wave digestion-cloud point extraction to come the method for cadmium content in booster flame aas determination rice to improve sensitivity and anti-matrix interference performance.
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 (7)
1. the method for trace amount of cadmium in a Flame Atomic Absorption Spectrometry Determination rice is characterized in that: comprise the following steps:
A. sample collection: commercially available rice is cleaned to the air-dry clean container of putting into, clean container is put into to temperature and at the constant temperature oven of 100 ℃, dry 2h, take out to be placed in and grind alms bowl and pulverize powdered, obtain rice sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. the sample micro-wave digestion is processed and is obtained sample solution: accurately take rice sample and be placed in clean dry teflon pressure dispelling tank, add and clear up solvent soaking and spend the night, the described solvent of clearing up is that massfraction is respectively 65% nitric acid 1mL, the mixed solvent of 30% hydrogen peroxide 3mL, prepare blank solution simultaneously, then seal and put into microwave digestion device according to micro-wave digestion program heating and decompose, after clearing up EOP (end of program), take out counteracting tank and be cooled to room temperature, shift sample to polytetrafluoroethylene beaker, beaker is placed in to low-temperature heat on electric hot plate and catches up with acid, until sample evaporation during to quick-drying, take off beaker cooling and shift test solution to volumetric flask, dilute constant volume with redistilled water, shake up and obtain sample solution, and under the environment of 6 ℃, preserve stand-by,
C. the preenrichment of sample cloud point extraction is processed and obtained testing sample solution: the sample solution quantitatively obtained in removing step b is in centrifuge tube, add the fully mixed hydrophobicity ionic associate that forms of complexing agent and sample solution, shake up the standing rear pH to 4.0 with damping fluid adjusting mixed solution ~ 5.0, then add 4.5% Triton-114 solution, obtain the non-ionic surfactant micelle solution, with redistilled water, it is diluted to constant volume, shake up to be placed in 40 ~ 60 ℃ of water-baths and be heated to cloud point temperature, centrifugal 10min(3800r/min while hot) make its phase-splitting, after the solution phase-splitting, ice bath is cooled to room temperature, remove the upper strata water, to the nital that adds 0.1mol/L in the rich micellar phase of lower floor, obtain testing sample solution,
D. standard solution preparation: take redistilled water as thinning agent, will be mixed with every titer the series standard solution of variable concentrations;
E. cadmium content in the Instrument measuring rice sample: described instrument comprises: flame atomic absorption spectrophotometer, cadmium hollow cathode lamp, and design parameter arranges as follows:
Analytical wavelengths: 228.8nm
Lamp current: 20mA
Spectral band-width: 0.4nm
Burner height: 5mm
Acetylene gas flow: 1.3 L/min
Air mass flow: air mass flow: 8.0mL/min
F. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, the drawing standard curve, according to the content of nickel in typical curve or regression equation calculation testing sample solution.
2. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 1, it is characterized in that: the volume of the addition of complexing agent described in step c is 40% ~ 50% of the sample solution amount of pipetting volume.
3. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 2 is characterized in that: the potpourri of the potassium iodide that the described complexing agent added in step c is the volume ratio 2mol/L that is 1:1 and the methyl green (MG) of 1.5mmol/L.
4. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 2, it is characterized in that: in step c, the volume of the addition of Triton-114 solution is 20% ~ 30% of described complexing agent addition volume.
5. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 1, it is characterized in that: the program of clearing up of setting in microwave digestion device in step b is staged intensification heating and decompose program, be specially, 200 ℃ of heating 5min, 220 ℃ of heating 5min, 240 ℃ of heating 10min, 200 ℃ of heating 5min.
6. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 5 is characterized in that: in step b, rice sample is 1:8.25 with the mass volume ratio g/mL that clears up solvent.
7. the method for trace amount of cadmium in Flame Atomic Absorption Spectrometry Determination rice according to claim 1 is characterized in that: in step c, for the damping fluid of regulating mixed solution pH, be the pH NaOH-potassium dihydrogen phosphate mixed liquor that is 4.0.
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| CN104677977A (en) * | 2015-03-27 | 2015-06-03 | 福州大学 | Method for measuring trace mercury and cadmium in water by cloud point extraction-inductively coupled plasma (ICP)-mass spectrometry (MS) combination |
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| CN106338477A (en) * | 2016-10-14 | 2017-01-18 | 内蒙古天奇中蒙制药股份有限公司 | Method for quick detection of contents of microelements in xuefuzhuyu pills |
| CN108072616A (en) * | 2016-11-17 | 2018-05-25 | 立邦涂料（中国）有限公司 | A kind of method of harmful heavy metal content in detection aqueous color paste |
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| CN108088804A (en) * | 2017-12-04 | 2018-05-29 | 武汉大学 | A kind of assay method of trace cadmium in water samples |
| CN110274882A (en) * | 2018-03-16 | 2019-09-24 | 福建省农业科学院农业质量标准与检测技术研究所 | Cadmium detrmination method in rice |
| CN108507862A (en) * | 2018-04-02 | 2018-09-07 | 福建省农业科学院农业质量标准与检测技术研究所 | A kind of Cadmium detrmination method in animal's liver |
| CN113406026A (en) * | 2021-06-15 | 2021-09-17 | 河北冀衡赛瑞化工有限公司 | Method for measuring content of potassium oxide in fertilizer by using flame atomic absorption spectrometer |
| CN114965322A (en) * | 2022-06-16 | 2022-08-30 | 中南大学 | Method for rapidly detecting heavy metal cadmium in rice |
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