CN114295609A - Kit and detection method for rapidly detecting heavy metals - Google Patents
Kit and detection method for rapidly detecting heavy metals Download PDFInfo
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- CN114295609A CN114295609A CN202210005415.2A CN202210005415A CN114295609A CN 114295609 A CN114295609 A CN 114295609A CN 202210005415 A CN202210005415 A CN 202210005415A CN 114295609 A CN114295609 A CN 114295609A
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Abstract
The invention relates to a kit, in particular to a kit and a detection method for rapidly detecting heavy metals, and belongs to the technical field of detection of heavy metals in food simulants. The kit consists of end covers and a shell, wherein the middle of the shell is divided into two independent reaction tanks which are not communicated by a partition plate, and the two end covers are respectively matched with the tops of the two reaction tanks and seal the two reaction tanks; the horizontal direction of casing is equipped with the screen cloth, and the screen cloth is two-layer about dividing into every reaction tank, and the lower floor space of screen cloth is used for placing the macroporous adsorbent resin who adsorbs the sodium sulfide. The method for rapidly detecting the heavy metal by using the kit is used for determining the heavy metal in food contact materials and food simulants of products.
Description
Technical Field
The invention relates to a kit, in particular to a kit and a detection method for rapidly detecting heavy metals, and belongs to the technical field of detection of heavy metals in food simulants.
Background
In the prior art, a colorimetric method is generally adopted for determining heavy metals in food simulants: 20mL of the food simulant test solution obtained by the migration test is sucked into a 50mL colorimetric tube, water is added to the colorimetric tube to reach the scale, 2mL of the standard use solution of lead with the concentration of 1mg/L is additionally taken into the 50mL colorimetric tube, 20mL of 4% acetic acid solution is added, and water is added to the scale to be uniformly mixed. And respectively adding 2 drops of sodium sulfide solution into the two solutions, standing for 5min after the two solutions are uniform, and comparing the colors of the simulant test solution and the standard solution.
When the method is used, the developer sodium sulfide solution needs to be prepared automatically, so that the detection time is long, and in the whole detection process, the sodium sulfide is hydrolyzed to generate hydrogen sulfide which volatilizes smelly eggs and is harmful to human bodies. And the sodium sulfide solution is easy to react with oxygen in the air, and the solution is easy to turn yellow, so that the prepared sodium sulfide solution cannot be stored for a long time.
Disclosure of Invention
The invention aims to provide a kit for rapidly detecting lead heavy metals, which can meet detection requirements, simplify detection steps, reduce the operation burden of testers and avoid the olfactory fatigue of the testers.
The invention also provides a method for rapidly detecting heavy metals by using the kit.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a kit for rapidly detecting heavy metals comprises end covers and a shell, wherein the middle of the shell is divided into two independent reaction tanks which are not communicated by a partition plate, and the two end covers are respectively matched with the tops of the two reaction tanks and seal the two reaction tanks; the horizontal direction of casing is equipped with the screen cloth, and the screen cloth is two-layer about dividing into every reaction tank, and the lower floor space of screen cloth is used for placing the macroporous adsorbent resin who adsorbs the sodium sulfide.
The rapid detection principle of the invention is that heavy metal (calculated by lead) in the food simulant test solution reacts with sodium sulfide in the macroporous adsorption resin to form yellow brown sulfide in an acid solution, and the yellow brown sulfide is compared with the color of a lead standard solution. The macroporous adsorption resin for adsorbing sodium sulfide is used as a color developing agent for reacting with lead, and can adsorb most hydrogen sulfide gas after color developing reaction.
Preferably, the two reaction tanks have the same structure, wherein one reaction tank is used for developing the color of the food simulant, and the other reaction tank is used for developing the color of the lead standard solution.
Preferably, the shell and the partition plate are made of PS transparent plastics. The shell is made of PS transparent plastic, so that the color phenomenon after color development reaction can be observed conveniently.
Preferably, the screen is a 50 mesh nylon screen. The acid-resistant nylon is selected as the screen mesh with the mesh number of 50, so that the adsorption resin can be prevented from being suspended in the food simulant to influence the observation of the color.
Preferably, the end caps are a polytetrafluoroethylene material. The end cover is made of acid-alkali-resistant polytetrafluoroethylene material, has certain sealing performance, and prevents odor of the smelly eggs from overflowing.
Preferably, the macroporous adsorbent resin is YKDX-4 type resin produced by Tianjin Kaishi resin science and technology Limited. The YKDX-4 type resin mainly comprises styrene polymer, and has a nonpolar, 400-m specific surface area2(ii)/g, average pore diameter is 65-76 nm.
Preferably, the preparation method of the macroporous adsorption resin for adsorbing sodium sulfide comprises the following steps: the mass ratio of the macroporous adsorption resin to the sodium sulfide solution is 2 g: 3mL, and removing the water solvent after uniformly mixing to obtain the macroporous adsorption resin for adsorbing the sodium sulfide.
The method for rapidly detecting the heavy metal by using the kit is used for determining the heavy metal in food contact materials and food simulators of products. The method is developed on the basis of the national standard GB 31604.9-2016. The invention analyzes whether the heavy metal migration amount (calculated by lead) in the food contact material and the product reaches the standard or not by comparing the color generation with the lead standard solution, does not need to prepare a sodium sulfide solution, can directly react with the color developing agent in the kit by the food simulant, has simple and convenient operation and improves the detection efficiency.
The technical difficulty of the invention is that: in order to realize the purpose of rapid detection, the key point is to simplify the operation process, and to use any medium as a sodium sulfide carrier without preparing a sodium sulfide solution, so that the sodium sulfide can be effectively preserved without influencing the subsequent color reaction, thereby becoming the technical difficulty of the detection method of the invention.
The invention is developed around the technical difficulty and how to simply operate:
1. selection of sodium sulfide adsorption carrier: from pH test paper inspiration, try to use test paper color development mode to judge fast, explore the influence of the test paper of different materials to sodium sulfide color development, the experiment finds because the existence of glycerine protectant, and the sodium sulfide solution is difficult to adsorb on the test paper and is difficult to dry, consuming time overlength. Then, different adsorption materials such as activated carbon, molecular sieve and resin are tried, and the adsorption and desorption capacity of the macroporous adsorption resin is found to be utilized, so that the sodium sulfide can be effectively adsorbed, and after the acidic food simulation liquid is added, the sodium sulfide can be desorbed to have obvious color reaction with heavy metal (lead) in the simulation liquid.
2. Selection of macroporous adsorption resin types: because the sodium sulfide solution is a mixed solution of glycerol and water, and the glycerol and the water are polar, polar and strong-polar resins of different manufacturers are selected for research, but experiments show that the polar resin cannot achieve an ideal color development effect, the experiments are trapped in a bottleneck, then thinking is changed, the polar range of the resin is expanded, screening is carried out from non-polar to polar, and finally the model YKDX-4 non-polar macroporous adsorption resin is selected.
3. The proportion of the macroporous adsorption resin and the sodium sulfide solution is selected as follows: how to fully utilize the surface adsorbability of the resin and not excess sodium sulfide solution, from the perspective of cost and environmental protection, through static adsorption test, the optimal ratio of the mass of the macroporous adsorption resin to the sodium sulfide solution is 2 g: 3 mL.
The invention also optimizes the materials of the shell, the filter screen and the end cover, wherein the shell is made of PS transparent plastic, the filter screen is made of acid-resistant nylon plastic, and the end cover is made of acid-resistant alkali-resistant tetrafluoroethylene plastic with sealing property, so as to achieve the aim of environmental protection.
The invention has the beneficial effects that: according to the invention, whether the heavy metal migration amount (calculated by lead) in the food contact material and the product reaches the standard is analyzed by comparing the color generation with that of the lead standard solution, a sodium sulfide solution is not required to be prepared, the food simulant can directly react with the color developing agent in the kit, the operation is simple and convenient, and the efficiency is improved; the tightness of the kit reduces the harm of hydrogen sulfide gas to human body and eliminates potential safety hazard.
The kit for rapidly detecting the heavy metal can be applied to food contact materials and products, and the determination test of the heavy metal in food simulants.
Drawings
FIG. 1 is a schematic structural diagram of a kit according to the present invention; description of reference numerals: 1, a shell, 2 end covers, 3 partition plates, 4 screens and 5 macroporous adsorption resins;
fig. 2 is a photograph showing the results of the resin validity verification test.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made to the invention without departing from the scope thereof.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Example (b):
a kind of kit for detecting heavy metal fast, its structure is shown as figure 1, this kit is made up of end cap 2 and body 1, the body is divided into two independent reaction tanks not communicated by the baffle 3 in the middle, two end caps cooperate with top of two reaction tanks separately and make it seal; the horizontal direction of casing is equipped with screen cloth 4, and the screen cloth is two-layer about dividing into every reaction tank, and the lower floor space of screen cloth is used for placing the macroporous absorbent resin 5 that adsorbs the sodium sulfide.
The two reaction tanks have the same structure, one reaction tank is used for developing the color of the food simulant, and the other reaction tank is used for developing the color of the lead standard solution.
In this embodiment, the shell is made of PS transparent plastic, the whole shell has a length of 4.4cm, a width of 2.2cm and a height of 8cm, and the middle is partitioned into two separate reaction tanks by a PS plastic plate with a thickness of 0.2 cm. The end cover is made of acid and alkali resistant polytetrafluoroethylene, the shape of the end cover adopts a flat top design, the distance between the top edge and the lower end edge is 0.1cm, and the end cover is attached to the wall thickness of the reaction tank; the lower end is 2cm and is consistent with the inner diameter of the reaction tank.
The preparation of the macroporous adsorption resin for adsorbing sodium sulfide in the kit for rapidly detecting heavy metals of the embodiment:
1. pretreatment of macroporous adsorption resin:
soaking the resin in 0.5BV of ethanol for 24h (1BV is 1 resin bed volume), passing 2BV of ethanol through the resin column at a flow rate of 2BV/h, soaking for 4-5 h, washing the resin with 2BV/h until the effluent is not white turbid, and washing with water at the same flow rate. And (3) passing a 5% (wt) HCl solution of 2B through the resin layer at a flow rate of 4-6 BV/h, and soaking the resin for 2-4 h. And then washing with water at the same flow rate until the pH of the effluent is neutral, passing 2BV of 2% (wt) NaOH solution through the resin layer at the flow rate of 4-6 BV/h, soaking the resin for 2-4 h, then washing with water at the same flow rate until the pH of the effluent is neutral, and removing water at low temperature for later use.
Preparing a sodium sulfide solution: 15.4g of sodium sulfide nonahydrate (Na) were weighed out2S·9H2O), adding 10mL of water, stirring thoroughly with a glass rod until dissolved, adding 30mL of glycerol, mixing, sealing and storing.
2. Filling macroporous adsorption resin:
the mass ratio of the macroporous adsorption resin to the sodium sulfide solution is 2 g: 3mL, and after mixing well, removing the aqueous solvent at low temperature. Weighing 0.5g of macroporous adsorption resin, spreading the macroporous adsorption resin on the bottom of the reaction tank, covering a 50-mesh nylon screen as a baffle, and fixing the macroporous adsorption resin at 1/4 of the reaction tank in a clamping groove manner.
In the resin effectiveness verification test, macroporous adsorption resins of different types for adsorbing sodium sulfide are placed for 20 days and then compared to verify the selection of the resins and the stability of the functions after adsorption.
In each test tube, 20mL of 1mg/L lead standard solution (matrix: 4% acetic acid) was used, sequence number 0 was used as a control (no resin was added, and an equivalent amount of sodium sulfide solution was directly added), sequence numbers 1 to 6 were used to compare different types of resins with sequence number 0, and the types and main parameters of the resins of sequence numbers 1 to 6 are shown in Table 1. The test results are shown in FIG. 2.
TABLE 1
As can be seen from FIG. 2, the numbers 1 and 0 are yellowish brown, the numbers 2, 6 and 4 are lighter in color, and the numbers 3 and 5 are transparent in color. From the reaction phenomenon, the polarity of the resin is a main factor influencing the adsorption effect, the nonpolar resin can effectively adsorb sodium sulfide, and the resin reacts with lead under an acidic condition to have a yellowish brown phenomenon, but the resin with smaller specific surface area and pore size has an obvious color development phenomenon, so that the resin with the type YKDX-4 is selected for detection.
Static adsorption test
A certain amount of resin is taken, and the sulfur content in the sodium sulfide solution during the addition and the sulfur content in the residual liquid after the adsorption are tested by adopting an inductively coupled plasma atomic emission spectrometry (ICP-OES method), so that the proportion is determined, and the detection result is shown in Table 2.
TABLE 2
As can be seen from Table 2, with the increase of the volume of the added sodium sulfide, the sulfur concentration in the residual solution after adsorption is changed to 1.5-2.0mL, which indicates that the sodium sulfide is saturated in the resin pores; and (3) subdividing the volume concentration gradient of the sodium sulfide, selecting 6 concentration points between 1.5 and 2.0, and performing experiments again to determine that the optimal ratio of the mass of the macroporous adsorption resin to the sodium sulfide solution is 2 g: 3 mL.
The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same or similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The kit and the detection method for rapidly detecting the heavy metal provided by the invention are described in detail above. The principles and embodiments of the present invention have been explained herein using specific examples, which are presented solely to aid in the understanding of the methods and their underlying concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A kit for rapidly detecting heavy metals is characterized in that: the kit consists of an end cover (2) and a shell (1), wherein the middle of the shell is divided into two independent reaction tanks which are not communicated by a partition plate (3), and the two end covers are respectively matched with the tops of the two reaction tanks and seal the two reaction tanks; the horizontal direction of casing is equipped with screen cloth (4), and the screen cloth is two-layer about dividing into every reaction tank, and the lower floor space of screen cloth is used for placing the macroporous adsorbent resin (5) that adsorbs the sodium sulfide.
2. The kit for rapidly detecting heavy metals according to claim 1, wherein: the two reaction tanks have the same structure, wherein one reaction tank is used for developing the color of the food simulant, and the other reaction tank is used for developing the color of the lead standard solution.
3. The kit for rapidly detecting heavy metals according to claim 1, wherein: the shell and the partition plate are made of PS transparent plastics.
4. The kit for rapidly detecting heavy metals according to claim 1, wherein: the screen is a 50-mesh nylon screen.
5. The kit for rapidly detecting heavy metals according to claim 1, wherein: the end cover is made of polytetrafluoroethylene materials.
6. The kit for rapidly detecting heavy metals according to claim 1, wherein: the main component of the macroporous adsorption resin is styrene polymer, which has non-polarity and specific surface area of 400-450m2(ii)/g, average pore diameter is 65-76 nm. Is YKDX-4 type resin produced by Tianjin Kaishi resin science and technology Limited.
7. The kit for rapidly detecting heavy metals according to claim 1, which is characterized in that the preparation method of the macroporous adsorption resin for adsorbing sodium sulfide comprises the following steps: the mass ratio of the macroporous adsorption resin to the sodium sulfide solution is 2 g: 3mL, and removing the water solvent after uniformly mixing to obtain the macroporous adsorption resin for adsorbing the sodium sulfide.
8. The kit for rapidly detecting heavy metals according to claim 7, wherein the sodium sulfide solution is prepared by the following steps: 15.4g of sodium sulfide nonahydrate (Na) were weighed out2S·9H2O), adding 10mL of water, stirring thoroughly with a glass rod until dissolved, adding 30mL of glycerol, mixing, sealing and storing.
9. A method for rapidly detecting a heavy metal using the kit of claim 1.
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| CN202210005415.2A CN114295609B (en) | 2022-01-05 | 2022-01-05 | Kit and method for rapidly detecting heavy metals |
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| JPH08285841A (en) * | 1995-04-19 | 1996-11-01 | Duskin Co Ltd | Method and kit for detecting guanine or acarid in dust |
| JP2007333689A (en) * | 2006-06-19 | 2007-12-27 | Hiroshi Yokozawa | Simple measurement kit |
| JP2008107264A (en) * | 2006-10-27 | 2008-05-08 | Fujitsu Ltd | Detection body and detection method |
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| CN112945950A (en) * | 2021-03-08 | 2021-06-11 | 唐山三友化工股份有限公司 | Limit analysis method for enriching heavy metals in food additive sodium carbonate by using microporous filter membrane |
| CN214622340U (en) * | 2021-04-14 | 2021-11-05 | 甘肃省药品检验研究院 | Heavy metal detection device based on colorimetric method |
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2022
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| US5550061A (en) * | 1989-02-02 | 1996-08-27 | Hybrivet Systems, Inc. | Test swab and method of using same |
| JPH08285841A (en) * | 1995-04-19 | 1996-11-01 | Duskin Co Ltd | Method and kit for detecting guanine or acarid in dust |
| JP2007333689A (en) * | 2006-06-19 | 2007-12-27 | Hiroshi Yokozawa | Simple measurement kit |
| JP2008107264A (en) * | 2006-10-27 | 2008-05-08 | Fujitsu Ltd | Detection body and detection method |
| CN103983642A (en) * | 2014-06-03 | 2014-08-13 | 三棵树涂料股份有限公司 | Sulfide-based metallic lead ion colorimetric detection method |
| CN112945950A (en) * | 2021-03-08 | 2021-06-11 | 唐山三友化工股份有限公司 | Limit analysis method for enriching heavy metals in food additive sodium carbonate by using microporous filter membrane |
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