CN115201289A - Heavy metal detection method based on screen printing electrode and detection instrument thereof - Google Patents
Heavy metal detection method based on screen printing electrode and detection instrument thereof Download PDFInfo
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- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- 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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- 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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Abstract
The invention discloses a heavy metal detection method based on a screen printing electrode and a detection instrument thereof, wherein the heavy metal detection method based on the screen printing electrode comprises the following steps: s1, preprocessing a sample; s2, detecting electrode activation treatment; s3, detecting a sample; and S4, data processing and result analysis printing. The invention relates to the technical field of food safety detection. The heavy metal detection method and the detection instrument based on the screen printing electrode have the characteristics of simple operation, quick detection, good stability and high accuracy, and are particularly suitable for quickly and quantitatively detecting the heavy metal in the grains.
Description
Technical Field
The invention belongs to the technical field of food safety detection, and relates to a method for quickly and efficiently detecting heavy metals such as cadmium, lead and the like in foods such as rice and the like.
Background
At present, there are many methods for detecting heavy metals in food, such as: in recent years, rapid detection technologies are rapidly developed, such as an enzyme analysis method, a biosensor analysis method, an X-ray fluorescence method, an immunoassay method and the like, and the rapid detection method is mature and can measure the content of heavy metals in a sample in a short time. However, the conventional sample pretreatment methods, such as dry ashing method, wet digestion, microwave digestion method, high-pressure digestion method, etc., all require a long treatment time, a large amount of acid reagents, a high-temperature and high-pressure environment or a heat setting instrument, and become bottlenecks in rapid detection and on-site detection of heavy metals in food.
The traditional pretreatment extraction method of inorganic elements in food mainly comprises a wet digestion method, a dry ashing method and a microwave digestion method.
The wet digestion method is to add strong oxidizing acid into food and to heat and boil at the same time to decompose and oxidize organic substances into CO 2 Water and various gases. Digestion is often accompanied by a large amount of acid mist and other toxic wastes, pollutes air, endangers the health of experimental operators, and is usually carried out in a fume hood, and digestion of one sample generally takes 4-5 hours. Sometimes, a high-pressure stewing pot is adopted for digestion, the sample and the strong acid are placed in the high-pressure stewing pot and placed in a baking oven for high-temperature high-pressure digestion, generally, the digestion is complete, more time is needed for one day after the sample and the strong acid are cooled overnight and then removed, and the sample and the strong acid can explode when the operation is improper.
The dry ashing method is that a certain amount of sample is placed in a crucible to be heated, organic matters in the sample are dehydrated, decomposed, oxidized and carbonized, then the sample is covered in a high-temperature electric furnace to be burnt and ashed until residues are white or light gray, the obtained residues are inorganic components, and the residual ash is dissolved by acid to be used as a sample solution to be detected. The ashing temperature is generally 500 ℃ to 600 ℃ and the digestion time is generally 4 to 8 hours. The sample containing much fat and sugar takes a long time. Some sulfur and nitrogen containing compounds produce corresponding oxides and exhaust gases pollute the air. Chlorinated hydrocarbon compounds not only pollute the air, but also corrode the ashing furnace.
The microwave digestion method is characterized in that a sample and digestion solution (usually nitric acid, hydrochloric acid, hydrofluoric acid, hydrogen peroxide and the like) are mixed in a special microwave digestion tank by adopting a microwave heating principle in a closed container, and the purpose of sample pretreatment is achieved under the conditions of high temperature and high pressure. As an efficient sample pretreatment method, microwave digestion can well meet the requirements of modern instrument analysis on the sample pretreatment process, and has the advantages of high heating speed, uniform heating, small reagent dosage, low blank, energy conservation, high efficiency and the like. However, active safety measures are required, including high-precision temperature and pressure control systems, pressure tank safety pressure relief systems, vertically oriented explosion-proof systems, high-strength explosion-proof safety doors and the like. The microwave digestion instrument is also required to be placed on a firm and stable test bed, the top and the left and the right of the furnace body are not covered, and gaps are reserved to keep good ventilation. The heating source should be avoided to avoid the fault caused by the hot water and steam entering the microwave oven, and the heating source should be kept away from the tap water source to avoid the electric leakage danger caused by the splashing. Do not come close to ferromagnetic materials or electrical appliances with magnetism because the external magnetic field interferes with the uniform distribution of the magnetic field in the furnace, which reduces heating efficiency, and requires other normal laboratory temperatures and hydroelectric conditions.
Although the classical methods can accurately extract the heavy metals in the sample, the classical methods are time-consuming, labor-consuming, complex in steps and high in requirements. The pretreatment in one process is less than 4-5 hours and more than ten hours, and the detection time of the instrument can detect the result within 5min of each sample of the graphite furnace atomic absorption instrument. Meanwhile, the methods generally consume more strongly corrosive acid and oxidizing reagent, need higher temperature, increase the risks of loss and pollution of the sample to be detected and the potential safety hazard of operators, and are difficult to adapt to the requirements of large-batch high-throughput green and environment-friendly rapid detection of the current sample.
Short, the little instrument of detection error has become the urgent demand of food production processing enterprises such as cereal and relevant units during the detection, will satisfy the market demand, how can be quick draw out heavy metal from food such as cereal and detect, just become the key problem for realizing short-term test or witnessed inspections.
Disclosure of Invention
The invention aims to provide a heavy metal detection method based on a screen printing electrode, which is characterized by comprising the following steps of:
s1, sample pretreatment: preparing a grain sample to be detected, adding a pretreatment solution into the grain sample to be detected for soaking, and taking clear liquid as a sample solution to be detected after full extraction;
s2, detection electrode activation treatment: preparing an activation treatment solution, adding the activation treatment solution into an analysis pool, and placing a detection electrode in the analysis pool for activation;
s3, sample detection: adding a proper amount of sample solution to be detected into an analysis pool, and detecting by using an activated electrode;
s4, data processing and result analysis printing: and (4) repeating the steps S2 and S3 to obtain a plurality of grain sample detection results to be detected, and processing and analyzing the data.
Further, in the step S1, the grain is selected from rice, brown rice, wheat or corn, the grain to be detected is firstly crushed to prepare a powder grain sample to be detected with the grain diameter of 0.12mm-0.85mm, and then the pretreatment liquid is added for soaking.
Further, the pretreatment liquid in the S1 comprises one or more of hydrochloric acid, nitric acid, sulfuric acid and acetic acid, the concentration is less than 6mol/L, and the addition amount is 3ml/g-10ml/g.
Further, adding the pretreatment liquid into the S1, oscillating for 2-5min, controlling the temperature to be 20-35 ℃, and standing or centrifuging or filtering to obtain clear liquid serving as a sample solution to be detected.
Further, the activation treatment solution in S2 comprises one or more of ammonium acetate, sodium acetate, mercury salt and bismuth salt, and the concentration is 0.2g/L-20g/L.
Further, in S2, 800 μ L of the activation treatment liquid was added to the analysis cell, and the screen-printed electrode was extended into the activation treatment liquid to perform the activation treatment of the working electrode.
Further, in the step S3, 200 μ L of the sample solution to be tested obtained in the step S1 is added to the analysis cell for detection after the activation treatment is finished.
Further, in the step S3, after the grain sample to be detected is detected, the heavy metal concentration of the grain sample to be detected is calculated and recorded according to the collected related data by a standard addition method, a standard curve built-in method or a field standard curve making method.
Further, in the step S4, a plurality of grain sample detection results to be detected are obtained, an average value and a CV value are calculated for the detection results, and the detection results and the calculation results are output in the form of a map or data.
Furthermore, the integrated heavy metal detection instrument used in the invention comprises a test module, a data acquisition module, a signal amplification processing module, a data processing and analyzing module and a result output printing module.
Further, lie in test module includes electrode plug fixing base, electrode installation plug, electrode insertion pilot lamp, screen printing electrode, lifter, analysis cell, rotatory section of thick bamboo and base, the lifter sets up the rear portion at the base, rotatory section of thick bamboo is established in the front portion of base, the analysis cell sets up the inside at rotatory section of thick bamboo, electrode plug fixing base articulates the upper end at the lifter, electrode installation plug is established in the front portion of electrode plug fixing base, screen printing electrode detachably is fixed in the electrode installation plug.
Furthermore, when detecting various elements, an electrolyte of the element to be detected can be prepared first, and the electrochemical characteristics of the element to be detected on the surface of the electrode are tested by cyclic voltammetry or linear scanning voltammetry, so that the qualitative oxidation and reduction potentials of various types of elements to be detected in a specific matrix are obtained correspondingly. Determining measurement parameters according to the obtained oxidation and reduction potentials, depositing trace elements to be detected in an enrichment solution on the surface of a screen printing electrode under different potentials, carrying out sectional oxidation dissolution on different types of elements to be detected deposited on the surface of the screen printing electrode, testing the oxidation dissolution curve graphs of standard solutions with different concentrations of the different types of elements to be detected, obtaining the linear working curve of the concentration of each element and the oxidation peak current value or the oxidation peak area, testing the oxidation dissolution curve of an actual sample of a food sample such as rice and the like containing any different concentrations and types of elements to be detected under the same testing condition, obtaining an oxidation peak current curve obtained by oxidizing the elements to be detected, comparing the oxidation peak current curve with the standard linear working curve, and obtaining the type and the concentration of the elements to be detected in the actual sample.
Furthermore, when the measurement of multiple elements is carried out, the quantitative oxidation dissolution curves of different types of elements can be respectively tested by adopting a multi-step method, namely, the element with the highest reduction potential is deposited firstly according to the sequence of the reduction potential from high to low, and then the scanning is carried out to obtain the quantitative oxidation dissolution curve of the deposited element, namely, only one element is deposited and measured each time by modifying the deposition potential and scanning parameters, so that the interference among the elements is avoided, and the accuracy of the test result is improved.
Compared with the prior art, the invention has the following effects:
(1) The pretreatment method mainly adopts low-concentration acid soaking, so that the condition that operators are possibly injured by contacting a large amount of concentrated acid is avoided;
(2) The extraction method of the invention is used for extracting the heavy metals in the grains, and the extraction process does not need high temperature and high pressure conditions, does not need specific instruments and is convenient to operate;
(3) The detection method can simultaneously extract various heavy metals, and the extraction process is completed within 30 minutes;
(4) The detection method adopts the plug-in type ready-to-use disposable silk screen printing electrode, has stable performance, omits the complicated process of traditional electrode polishing and maintenance, and can improve the sensitivity and the precision of detection by activating the electrode before detection.
Drawings
The invention is described in further detail below with reference to the following figures and detailed description:
fig. 1 is a schematic diagram of steps of a heavy metal detection method based on a screen printing electrode.
Fig. 2 is a schematic diagram of the working principle of the heavy metal detection instrument based on the screen printing electrode.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure of the present invention.
Please refer to fig. 1. It should be understood that the structures, ratios, sizes, etc. shown in the drawings and attached to the description are only for understanding and reading the disclosure of the present invention, and are not intended to limit the practical conditions of the present invention, so that the present invention has no technical significance, and any modifications of the structures, changes of the ratio relationships, or adjustments of the sizes, should still fall within the scope of the technical contents of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
Example 1: the method for detecting the concentration of heavy metals in rice comprises the following steps:
(1) Taking 200g of a representative rice sample, and crushing the representative rice sample by a crusher to prepare a powder sample with the particle size of 0.630 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 5 mL of sulfuric acid pretreatment liquid with the concentration of 4mol/L, and manually shaking for 5min;
(3) Standing for 5min, and taking supernatant to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises ammonium acetate (0.2-10 g/L), sodium acetate (0.2-10 g/L), and mercuric sulfate (0.2-0.5 g/L) with total concentration of 15 g/L), placing the analysis cell in a rotary barrel of a test instrument; and taking out the disposable screen printing electrode, inserting the disposable screen printing electrode into the electrode mounting plug, pressing down the electrode, and clicking an electrode activation button on a detection interface of the portable heavy metal detector to activate the electrode. And after the electrode activation is finished, adding 200 mu L of supernatant to be detected into the analysis cell, and clicking a test button of a detection interface to detect the sample. After the detection is finished, clicking a report button of a detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 1.
TABLE 1 detection results of heavy metal cadmium in rice
Example 2: the method for detecting the concentration of heavy metals in rice comprises the following steps:
(2) Taking 200g of a representative rice sample, and crushing the representative rice sample by a crusher to prepare a powder sample with the particle size of 0.850 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 5 mL of nitric acid pretreatment liquid with the concentration of 6mol/L, and placing on a vortex instrument to shake for 2min;
(3) Centrifuging at 5000rpm for 5min, and collecting clear liquid to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises ammonium acetate (0.2-10 g/L), sodium acetate (0.2-10 g/L), and mercuric sulfate (0.2-0.5 g/L) with total concentration of 15 g/L), placing the analysis cell in a rotary barrel of a test instrument; and taking out the disposable screen printing electrode, inserting the disposable screen printing electrode into the electrode mounting plug, pressing down the electrode, and clicking an electrode activation button on a detection interface of the portable heavy metal detector to activate the electrode. After electrode activation was complete, 200. Mu.L of the assay supernatant was added to the cell. Clicking a test button of a detection interface to detect a sample; and after the detection is finished, clicking a report button of the detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 2.
Table 2 detection results of heavy metal cadmium in rice
Example 3: the method for detecting the concentration of heavy metals in rice comprises the following steps:
(3) Taking 200g of a representative rice sample, and crushing the representative rice sample by a crusher to prepare a powder sample with the particle size of 0.125 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 3mL of sulfuric acid pretreatment solution with the concentration of 4mol/L, and placing on a vortex instrument to shake for 4min;
(3) Centrifuging at 5000rpm for 5min, and collecting clear liquid to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises sodium acetate (0.2-10 g/L), mercury sulfate (0.2-0.5 g/L), bismuth sulfate (0.2-0.5 g/L) and total concentration is 10 g/L), and placing the analysis cell into a rotary barrel of a test instrument; and taking out the disposable screen printing electrode, inserting the disposable screen printing electrode into the electrode mounting plug, pressing down the electrode, and clicking an electrode activation button on a detection interface of the portable heavy metal detector to activate the electrode. And after the electrode activation is finished, adding 200 mu L of supernatant to be detected into the analysis cell, and clicking a test button of a detection interface to detect the sample. After the detection is finished, clicking a report button of the detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 3.
TABLE 3 detection results of heavy metal cadmium in rice
Example 4: the method for detecting the concentration of the heavy metal in the rice comprises the following steps:
(1) Taking 150g of a representative rice sample, carrying out hulling treatment on the rice, and crushing the rice by a crusher to prepare a powder sample with the particle size of 0.425 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 5 mL of sulfuric acid pretreatment solution with the concentration of 4mol/L, and placing on a vortex instrument to shake for 4min;
(3) Centrifuging at 3000rpm for 2min, and collecting clear liquid to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises ammonium acetate (0.2-10 g/L), sodium acetate (0.2-10 g/L), bismuth sulfate (0.2-0.5 g/L), and total concentration is 15 g/L), placing the analysis cell in a rotary barrel of a test instrument, taking out the disposable silk screen printing electrode, inserting into an electrode mounting plug, pressing down the electrode, and clicking an electrode activation button of a detection interface of a portable heavy metal detector to activate the electrode. And after the electrode activation is finished, 200 mu L of supernatant to be detected is added into the analysis cell, and a test button of a detection interface is clicked to detect the sample. After the detection is finished, clicking a report button of the detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 4.
TABLE 4 detection results of heavy metal cadmium in rice
| Serial number | Cadmium concentration (mg/kg) | Original current (μ A) |
| 1 | 0.169 | 0.2582 |
| 2 | 0.168 | 0.2567 |
| 3 | 0.165 | 0.2519 |
| 4 | 0.168 | 0.2582 |
| 5 | 0.165 | 0.2567 |
| 6 | 0.166 | 0.2519 |
| Mean value of | 0.167 | 0.2556 |
| CV value | 1.03％ |
Example 5: the method for detecting the concentration of the heavy metal in the wheat comprises the following steps:
(1) Taking 100g of a representative wheat sample, and crushing the representative wheat sample by a crusher to prepare a powder sample with the particle size of 0.630 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 5 mL of hydrochloric acid pretreatment liquid with the concentration of 6mol/L, and placing on a vortex instrument to shake for 5min;
(3) Centrifuging at 3000rpm for 3min, and collecting clear liquid to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises ammonium acetate (0.2-10 g/L), sodium acetate (0.2-10 g/L), bismuth sulfate (0.2-0.5 g/L), and total concentration is 18 g/L), placing the analysis cell in a rotary barrel of a test instrument, taking out the disposable silk screen printing electrode, inserting into an electrode mounting plug, pressing down the electrode, and clicking an electrode activation button of a detection interface of a portable heavy metal detector to activate the electrode. And after the electrode activation is finished, 200 mu L of supernatant to be detected is added into the analysis cell, and a test button of a detection interface is clicked to detect the sample. And after the detection is finished, clicking a report button of the detection interface, checking the result and the detection report, and repeatedly detecting the sample for 6 times, wherein the test results are shown in the following table 5.
TABLE 5 detection results of heavy metal cadmium in wheat
| Number of | Cadmium concentration (mg/kg) | Original current (μ A) |
| 1 | 0.0540 | 0.1044 |
| 2 | 0.0512 | 0.0983 |
| 3 | 0.0540 | 0.1042 |
| 4 | 0.0530 | 0.1043 |
| 5 | 0.0520 | 0.1058 |
| 6 | 0.0536 | 0.1009 |
| Mean value of | 0.0530 | 0.1030 |
| CV | 2.2％ |
Example 6: the method for detecting the concentration of the heavy metal in the corn comprises the following steps:
(1) Taking 200g of a representative corn sample, and crushing the representative corn sample by a crusher to prepare a powder sample with the particle size of 0.42 mm;
(2) Respectively weighing 1.0g of each sample in the step (1) into a 10mL centrifuge tube, adding 5 mL of nitric acid pretreatment solution with the concentration of 5mol/L, and placing on a vortex instrument to shake for 5min;
(3) Centrifuging at 3000rpm for 3min, and collecting clear liquid to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment solution (the treatment solution comprises ammonium acetate (0.2-10 g/L), sodium acetate (0.2-10 g/L), bismuth sulfate (0.2-0.5 g/L), and total concentration is 20 g/L), placing the analysis cell in a rotary barrel of a test instrument, taking out the disposable silk screen printing electrode, inserting into an electrode mounting plug, pressing down the electrode, and clicking an electrode activation button of a detection interface of a portable heavy metal detector to activate the electrode. And after the electrode activation is finished, adding 200 mu L of supernatant to be detected into the analysis cell, and clicking a test button of a detection interface to detect the sample. After the detection is finished, clicking a report button of the detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 6.
TABLE 6 detection results of heavy metal cadmium in corn
| Number of | Cadmium concentration (mg/kg) | Original current (μ A) |
| 1 | 0.0430 | 0.0803 |
| 2 | 0.0440 | 0.0752 |
| 3 | 0.0420 | 0.0805 |
| 4 | 0.0420 | 0.0816 |
| 5 | 0.0420 | 0.0795 |
| 6 | 0.0410 | 0.0753 |
| Mean value of | 0.0423 | 0.0787 |
| CV | 2.4％ |
Example 7: the method for detecting the concentration of heavy metals in rice comprises the following steps:
(1) Taking 200g of a representative rice sample, putting the representative rice sample into a 20mL centrifuge tube, adding 5 mL of nitric acid pretreatment liquid with the concentration of 5mol/L, and placing the mixture on a vortex instrument to shake for 5min;
(3) Standing, and taking supernate to be tested;
(4) Taking out the analysis cell, adding 800 μ L of activation treatment liquid (the treatment liquid comprises ammonium acetate (0.2 g/L-10 g/L), sodium acetate (0.2 g/L-10 g/L), bismuth sulfate (0.2 g/L-0.5 g/L), and total concentration is 12 g/L), putting the analysis cell into a rotary barrel of a test instrument, taking out a disposable silk screen printing electrode, inserting into an electrode mounting plug, pressing down the electrode, and clicking an electrode activation button on a detection interface of a portable heavy metal detector to activate the electrode. And after the electrode activation is finished, 200 mu L of supernatant to be detected is added into the analysis cell, and a test button of a detection interface is clicked to detect the sample. After the detection is finished, clicking a report button of the detection interface, checking a result and a detection report, and repeatedly detecting the sample for 6 times, wherein the test result is shown in the following table 7.
Table 7 detection results of heavy metal cadmium in rice
| Numbering | Cadmium concentration (mg/kg) | Original current (μ A) |
| 1 | 0.1790 | 2.5302 |
| 2 | 0.1699 | 2.4295 |
| 3 | 0.1710 | 2.4451 |
| 4 | 0.1742 | 2.6818 |
| 5 | 0.1601 | 2.4716 |
| 6 | 0.1623 | 2.4988 |
| Mean value of | 0.1694 | 2.5095 |
| CV | 4.2％ | 3.7％ |
Example 8: the method for detecting the concentration of heavy metals in rice comprises the following steps:
(1) Taking 200g of a representative rice sample, putting the representative rice sample into a 20mL centrifuge tube, adding 5 mL of nitric acid pretreatment liquid with the concentration of 4mol/L, and placing the mixture on a vortex instrument to shake for 5min;
(3) Standing, and taking supernate to be tested;
(4) And taking out the analysis cell, adding 800 mu L of activation treatment solution with the concentration of 0.8g/L ammonium acetate, putting the analysis cell into a rotary barrel of a test instrument, taking out the disposable screen printing electrode, inserting the disposable screen printing electrode into an electrode mounting plug, pressing down the electrode, clicking an electrode activation button on a detection interface of the portable heavy metal detector, and carrying out electrode activation. And after the electrode activation is finished, adding 200 mu L of supernatant to be detected into the analysis cell, and clicking a test button of a detection interface to detect the sample. And after the detection is finished, clicking a report button of the detection interface, checking the result and the detection report, and repeatedly detecting the sample for 6 times, wherein the test results are shown in the following table 7.
TABLE 8 detection results of heavy metal cadmium in rice
| Numbering | Cadmium concentration (mg/kg) | Original current (μ A) |
| 1 | 0.0650 | 0.0879 |
| 2 | 0.0640 | 0.0859 |
| 3 | 0.0640 | 0.0862 |
| 4 | 0.0590 | 0.082 |
| 5 | 0.0580 | 0.0811 |
| 6 | 0.0610 | 0.0829 |
| Mean value of | 0.0620 | 0.08 |
| CV | 4.7％ | 1.3％ |
Example 9:
the sample prepared in example 4 was tested by using three instruments, namely a portable electrochemical heavy metal tester, a portable atomic emission element analyzer and a portable spectrophotometer, for 6 times, and the test data are as follows in table 9:
TABLE 9 comparison of the results of three types of instruments
From the above table data, it follows that: the CV value of the data detected by the portable electrochemical detector is smaller than that detected by an X-ray fluorescence spectrometry and an atomic absorption spectrophotometer, and the stability of the detection result is higher.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (13)
1. A heavy metal detection method based on a screen printing electrode is characterized by comprising the following steps:
s1, sample pretreatment: preparing a grain sample to be detected, adding a pretreatment solution into the grain sample to be detected for soaking, and taking clear liquid as a sample solution to be detected after full extraction;
s2, detecting electrode activation treatment: preparing an activation treatment solution, adding the activation treatment solution into an analysis pool, and placing a detection electrode in the analysis pool for activation;
s3, sample detection: adding a sample solution to be detected into an analysis pool, and detecting by using an activated electrode;
s4, data processing and result analysis printing: and (5) repeating the steps S2 and S3 to obtain a plurality of grain sample detection results to be detected, and processing, analyzing and printing the results.
2. The method for detecting the heavy metal based on the screen printing electrode according to claim 1, wherein in the step S1, the grain is selected from rice, brown rice, wheat or corn, the grain to be detected is firstly crushed to be prepared into a powdery grain sample to be detected with the grain diameter of 0.12mm-0.85mm, and then the pretreatment solution is added for soaking.
3. The heavy metal detection method based on the screen-printed electrode according to claim 1, wherein in S1, the pretreatment liquid comprises one or more of hydrochloric acid, nitric acid, sulfuric acid and acetic acid, the concentration of the pretreatment liquid is less than 6mol/L, and the addition amount is 3ml/g-10ml/g.
4. The method for detecting the heavy metal based on the screen printing electrode as claimed in claim 1, wherein the pretreatment liquid is added into the S1, then the oscillation is carried out for 2-5min, the temperature is controlled to be 20-35 ℃, and then the solution is kept still or centrifuged or filtered to obtain clear liquid as a sample solution to be detected.
5. The heavy metal detection method based on the screen printing electrode as claimed in claim 1, wherein the activation treatment liquid in S2 comprises one or more of ammonium acetate, sodium acetate, mercury salt and bismuth salt, and the concentration is 0.2g/L-20g/L.
6. The method for detecting heavy metal based on the screen-printed electrode as claimed in claim 1, wherein in the step S2, 800 μ L of the activation treatment solution is added into the analysis cell, and the screen-printed electrode is extended into the activation treatment solution to perform the activation treatment of the working electrode.
7. The method for detecting heavy metal based on screen printing electrode of claim 6, wherein in the step S3, 200 μ L of the sample solution to be detected obtained in the step S1 is added into the analysis cell for detection after the activation treatment is finished.
8. The heavy metal detection method based on the screen printing electrode of claim 7, wherein in the step S3, after the grain sample to be detected is detected, the collected related data is used for calculating and recording the heavy metal concentration of the grain sample to be detected by a standard addition method or a standard curve built-in method.
9. The method for detecting heavy metals based on screen printing of electrodes as claimed in claim 8, wherein in S4, a plurality of grain samples to be detected are obtained, an average value and CV value of the detection results are calculated, and the detection results and the calculation results are outputted in the form of a graph or data.
10. The heavy metal detection instrument based on the screen printing electrode is characterized by comprising a test module, a data acquisition module, a signal amplification processing module, a data processing and analyzing module and a result output printing module.
11. The heavy metal detecting instrument based on the screen-printed electrode as claimed in claim 10, wherein the testing module comprises an electrode plug fixing seat, an electrode mounting plug, an electrode insertion indicator lamp, a screen-printed electrode, a lifting rod, an analysis tank, a rotary cylinder and a base, the lifting rod is arranged at the rear part of the base, the rotary cylinder is arranged at the front part of the base, the analysis tank is arranged inside the rotary cylinder, the electrode plug fixing seat is hinged at the upper end of the lifting rod, the electrode mounting plug is arranged at the front part of the electrode plug fixing seat, and the screen-printed electrode is detachably fixed in the electrode mounting plug.
12. The heavy metal detection instrument based on the screen-printed electrode as claimed in claim 10, wherein the testing module is configured to perform detection of a plurality of elements, first, prepare an electrolyte of an element to be detected, test electrochemical characteristics of the element to be detected on the surface of the electrode by cyclic voltammetry or linear sweep voltammetry, correspondingly obtain qualitative oxidation and reduction potentials of each type of element to be detected in a specific matrix, and determine measurement parameters according to the obtained oxidation and reduction potentials; depositing trace elements to be detected in the enriched solution on the surface of the screen printing electrode under different potentials, oxidizing and dissolving different types of elements to be detected deposited on the surface of the screen printing electrode in a segmented manner, testing the oxidation dissolution curve of standard solutions with different concentrations of different types of elements to be detected, and obtaining a linear working curve of the concentration of each element and the oxidation peak current value or the oxidation peak area; and finally, testing the oxidation dissolution curve of the actual sample of the food sample containing the elements to be detected with any different concentrations and types under the same test condition to obtain an oxidation peak current curve obtained by oxidizing the elements to be detected, and comparing the oxidation peak current curve with the standard linear working curve so as to obtain the type and the concentration of the elements to be detected in the actual sample.
13. The heavy metal detection instrument based on the screen printing electrode as claimed in claim 10, wherein when the test module performs measurement of a plurality of elements, the test module further adopts a multi-step method to test quantitative oxidation dissolution curves of different types of elements respectively.
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