CN112683889B - Binary chromogenic test paper and method for rapidly and semi-quantitatively detecting Cd (II) - Google Patents
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Abstract
The invention discloses a binary color-developing test paper and a method for rapidly and semi-quantitatively detecting Cd (II), wherein the binary color-developing test paper for Cd (II) is prepared by taking PAN and dithizone (Dz) as composite color-developing agents and attaching the composite color-developing agents to medium-speed filter paper; preparing a binary color development type test paper standard colorimetric plate; the purpose of selectively and rapidly measuring Cd (II) is achieved by regulating and controlling the type and the dosage of the masking agent. The method has the advantages of simple operation, wide color development range, high accuracy, convenience in carrying and storage, widening the detection range of the test paper method for Cd (II) and the like.
Description
Technical Field
The invention belongs to the technical field of test paper preparation and application, relates to a preparation method of semi-quantitative test paper for Cd (II), and further relates to a method for detecting the content of Cd (II).
Background
With the rapid development of industries such as mining and metallurgy, the heavy metal ions in the environment are increasing. Mineral wastewater contains a large amount of heavy metal ions, such as Pb (II) and Cd (II), which continuously migrate to surface water and underground water over time. Cd (II) is a common heavy metal ion in water, has strong toxicity to biological communities in water, and finally enters a human body through the layer-by-layer accumulation of food chain action, thereby causing serious damage to the heart, liver and bone tissues of the human body; in addition, cd (II) has the characteristics of strong enrichment and difficult degradation, so that the research of sensitive detection of low-concentration Cd (II) is very important.
Patent CN103969258A discloses a test paper and method for rapid detection of Cd (II) by naked eyes, and although the operation technical requirement is low and the on-site detection is convenient, the color development range is 1 × 10 -6 ～1×10 -2 mol·L -1 For Cd (II) concentrations below 1X 10 -6 mol·L -1 The water sample cannot be subjected to color development and quantification; patent CN111307778A discloses a method for preparing copper ion semi-quantitative test paper and a detection method, but the test paper has complicated preparation steps and needs vacuum drying. Therefore, it is necessary to develop a detection method with simple operation, wide color development range and high accuracy.
Disclosure of Invention
Aiming at the defect that the color development range of the current test paper method for Cd (II) is narrow, the invention aims to provide a binary color development test paper and a method for rapidly and semi-quantitatively detecting Cd (II), wherein the method has the advantages of simple operation, wide color development range, high accuracy, convenient use of the test paper, convenience in carrying and storage, widened detection range of the test paper method for Cd (II) and the like.
The invention is realized by the following technical scheme.
A method for rapidly and semi-quantitatively detecting Cd (II) by using binary color-developing test paper comprises the following steps:
step 1, preparing PAN/Dz binary color-developing test paper
Mixing a PAN (1- (2-pyridylazo) -2 naphthol) chloroform solution and a Dz (dithizone) chloroform solution according to a mass ratio of 0.3/0.2 to prepare a PAN/Dz chloroform solution binary color developing agent, soaking the test paper in the PAN/Dz chloroform solution binary color developing agent, taking out the test paper after a certain time, and drying to obtain a binary color developing type test paper;
step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing a series of concentration gradient Cd (II) solutions, dropwise adding the solutions on the binary color-developing test paper prepared in the step (1), developing for a certain time, sucking the residual Cd (II) solutions by using absorbent paper, drying, inspecting and taking reaction fragments to prepare a PAN/Dz binary color-developing test paper standard colorimetric plate;
step 3, detecting Cd (II) solution with unknown concentration
And (3) adjusting the pH value of the Cd (II) solution to be detected, respectively adding a masking agent, dropwise adding the Cd (II) solution to be detected onto the binary color-developing test paper prepared in the step (1), detecting the color change, comparing the color change with the standard colorimetric plate prepared in the step (2), and carrying out semi-quantitative determination on the concentration of the Cd (II) solution to be detected.
With respect to the above technical solutions, the present invention has a further preferable solution:
preferably, in the step 1, the test paper is medium-speed qualitative filter paper, is soaked in a PAN/Dz chloroform solution for 30-60 min, is taken out, and is dried in an oven at 40-60 ℃.
Preferably, in the step 1, the mass concentration of the PAN chloroform solution is 0.003 to 0.015%, and the mass concentration of the Dz chloroform solution is 0.0015 to 0.0075%.
Preferably, in the step 2, the color development time is 30 to 90 seconds.
Preferably, in the step 3, the pH value of the Cd (II) solution to be detected is adjusted to 5-8.
Preferably, in the step 2, the concentration ranges of the series Cd (II) standard solutions are respectively 8.90X 10 -7 ～8.90×10 -4 mol·L -1 。
Preferably, in the step 3, the masking agent comprises the following raw materials in parts by mass:
2-6 parts of thiourea, 2-6 parts of phenanthroline, 2-9 parts of citric acid and 13-26 parts of thioglycolic acid.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1) The binary color-developing test paper and the method for rapidly and semi-quantitatively detecting Cd (II) provided by the invention have the advantages that the color development and inspection time is 30-90 s, the time consumption is short, and the method is an ideal rapid determination method.
2) The binary color-developing test paper and the method for rapidly and semi-quantitatively detecting Cd (II) provided by the invention can be used for detecting Cd (II) with the concentration of 8.90 multiplied by 10 -7 ～8.90×10 -4 Semi-quantitative detection of Cd (II) between mol/L is realized, and LOD is 8.90 multiplied by 10 -7 mol/L。
3) Compared with a precious detection instrument used in a laboratory, the binary chromogenic test paper and the method for rapidly detecting Cd (II) in a semi-quantitative manner have the advantages of low equipment requirement, simple operation method, wide chromogenic range, high accuracy and convenience for field detection.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIGS. 1 (a) and 1 (b) are UV-VIS absorption spectra before and after the complexation of PAN (a), dz (b) and Cd (II), respectively;
FIG. 2 is a standard colorimetric plate of PAN/Dz binary colorimetric cadmium test paper.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
The embodiment of the invention provides binary chromogenic test paper and a method for quickly and semi-quantitatively detecting Cd (II), which comprise the following steps:
step 1, preparing PAN (1- (2-pyridylazo) -2 naphthol)/Dz (dithizone) binary color-developing test paper.
Mixing the PAN chloroform solution and the Dz chloroform solution according to the mass ratio of 0.3/0.2 to prepare the PAN/Dz chloroform solution binary color developing agent, wherein the mass concentration of the PAN chloroform solution is 0.003-0.015 percent, and the mass concentration of the Dz chloroform solution is 0.0015-0.0075 percent; immersing the disc type medium-speed qualitative filter paper with the diameter of 6mm in the medium-speed qualitative filter paper, immersing the disc type medium-speed qualitative filter paper in a PAN/Dz chloroform solution for 30-60 min, taking out the disc type medium-speed qualitative filter paper, and drying the disc type medium-speed qualitative filter paper in an oven at the temperature of 40-60 ℃ to obtain the binary color development type test paper.
FIGS. 1 (a) and 1 (b) show the UV-VIS absorption spectra before and after complexation of PAN, dz and Cd (II). PAN and Dz are mixed to be a composite color developing agent, so that the color change of the reaction is enhanced on one hand, and the semi-quantitative detection range of Cd (II) by the composite color developing agent is widened on the other hand.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing serial Cd (II) solutions with concentration gradient of 8.90X 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the reagent solution on the binary color-developing test paper prepared in the step (1), developing for 30-90 s, sucking the residual Cd (II) solution by using absorbent paper, drying, inspecting and taking reaction fragments to prepare a PAN/Dz binary color-developing test paper standard colorimetric plate.
FIG. 2 shows a standard colorimetric plate of PAN/Dz binary colorimetric cadmium test paper.
Step 3, detecting Cd (II) solution with unknown concentration
Adjusting the pH value of the Cd (II) solution to be detected to 5-8, and respectively adding a masking agent for eliminating the interference of other coexisting ions, wherein the masking agent comprises the following raw materials in parts by mass: 2 to 6 portions of thiourea, 2 to 6 portions of phenanthroline, 2 to 9 portions of citric acid and 13 to 26 portions of thioglycolic acid.
And (3) transferring the solution of Cd (II) to be detected by using a rubber-tipped dropper, dripping the solution of Cd (II) to be detected onto the test paper prepared in the step (1), detecting the color change, comparing the color change with the standard colorimetric plate prepared in the step (2), and carrying out semi-quantitative determination on the concentration of the Cd (II).
The invention is further illustrated by the following different examples.
Example 1: detection of Cd (II) concentration in unknown water sample 1
Step 1, preparing PAN/Dz binary color-developing test paper
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.005%, and the mass concentration of the Dz chloroform solution is 0.0075%; and soaking the disc-shaped test paper with the diameter of 6mm in the test paper, taking out the test paper after 30min, and drying the test paper in a 60 ℃ oven to obtain the binary chromogenic test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing series Cd (II) solutions with concentration ranges of 8.90 × 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the test paper into the binary color-developing test paper prepared in the step (1), developing for 30s, sucking the residual Cd (II) solution with absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
Step 3, detecting Cd (II) solution with unknown concentration
Adjusting the pH value of a Cd (II) solution to be detected to be 7, and respectively adding a masking agent, wherein the masking agent comprises the following raw materials in parts by mass: 6 parts of thiourea, 5 parts of phenanthroline, 7 parts of citric acid and 20 parts of thioglycolic acid.
Taking a group of water samples to carry out three times of parallel experiments, transferring a Cd (II) solution to be detected (the pH value is 7) by using a rubber-tipped dropper, dripping the Cd (II) solution to be detected onto the test paper prepared in the step 1, inspecting the color change, comparing the color change with the standard colorimetric plate prepared in the step 2, and carrying out semi-quantitative determination on the concentration of the Cd (II) solution.
The colorimetric result shows that the concentration of Cd (II) in the solution is 4.45 multiplied by 10 -6 ～8.90×10 -6 Between mol/L. The data obtained by ICP examination were 7.36X 10, respectively -6 mol/L, and color comparisonThe result range obtained after the plate comparison is consistent, and the colors displayed among three groups of parallel samples are also the same, which shows that the test paper has good accuracy and stability.
Example 2: detection of Cd (II) concentration in unknown water sample 2
Step 1, preparing PAN/Dz binary color-developing test paper
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.0075%, and the mass concentration of the Dz chloroform solution is 0.003%; and soaking the circular test paper with the diameter of 6mm in the test paper, taking out the circular test paper after 40min, and drying the circular test paper in a 50 ℃ oven to obtain the binary color development test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing serial Cd (II) solutions with concentration gradient of 8.90X 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the test paper into the binary color-developing test paper prepared in the step (1), developing for 40s, sucking the residual Cd (II) solution by using absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
Step 3, detecting Cd (II) solution with unknown concentration
Adjusting the pH value of the Cd (II) solution to be detected to 7, and respectively adding a masking agent, wherein the masking agent comprises the following raw materials in parts by weight: 4 parts of thiourea, 6 parts of phenanthroline, 8 parts of citric acid and 13 parts of thioglycolic acid.
Taking a group of water samples to carry out three times of parallel experiments, transferring a Cd (II) solution to be detected (the pH value is 7) by using a rubber-tipped dropper, dripping the Cd (II) solution to be detected onto the test paper prepared in the step 1, inspecting the color change, comparing the color change with the standard colorimetric plate prepared in the step 2, and carrying out semi-quantitative determination on the concentration of the Cd (II) solution.
The colorimetric result shows that the concentration of Cd (II) in the solution is 4.45 multiplied by 10 -6 ～8.90×10 -6 Between mol/L. The data obtained by ICP examination were 4.59X 10, respectively -6 And the mol/L is consistent with the range of the result obtained after the comparison with a colorimetric plate, and the colors displayed among the three groups of parallel samples are also the same, which shows that the test paper has good accuracy.
Example 3: detection of Cd (II) concentration in simulated water sample 1
Step 1, preparing PAN/Dz binary color-developing test paper.
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.003 percent, and the mass concentration of the Dz chloroform solution is 0.0015 percent; and soaking the disc-shaped test paper with the diameter of 6mm in the test paper, taking out the test paper after 50min, and drying the test paper in a drying oven at 40 ℃ to obtain the binary chromogenic test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing series Cd (II) solutions with concentration ranges of 8.90 × 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the reagent solution on the binary color-developing test paper prepared in the step (1), developing for 80s, sucking the residual Cd (II) solution by using absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
In the step 3, interference ions such as Zn (II), cu (II) and the like are contained in the simulated water sample, and a masking agent for eliminating the interference of other coexisting ions is added into the water sample before the water sample is transferred, wherein the masking agent is 4 parts of thiourea, 6 parts of phenanthroline, 9 parts of citric acid and 13 parts of thioglycolic acid.
Semi-quantitative detection is carried out by utilizing binary chromogenic test paper, and the result is 4.45 multiplied by 10 -4 ～8.90×10 -4 Between mol/L, the data obtained by ICP examination was 5.21X 10 -4 And the mol/L is consistent with the range of the result obtained after the comparison with the colorimetric plate, and the colors displayed among the three groups of parallel samples are also the same, which shows that the test paper has better accuracy.
Example 4: detection of Cd (II) concentration in simulated water sample 2
Step 1, preparing PAN/Dz binary color development type test paper.
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.025 percent, and the mass concentration of the Dz chloroform solution is 0.0035 percent; and soaking the disc-shaped test paper with the diameter of 6mm in the test paper, taking out the test paper after 40min, and drying the test paper in a 55 ℃ oven to obtain the binary chromogenic test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing series Cd (II) solutions with concentration ranges of 8.90 × 10 -5 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the test paper into the binary color-developing test paper prepared in the step (1), developing for 75s, sucking the residual Cd (II) solution with absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
In the step 3, interference ions such as Zn (II), cu (II) and the like are contained in the simulated water sample, and a masking agent for eliminating interference of other coexisting ions is added into the water sample before the water sample is transferred, wherein the masking agent comprises 5 parts of thiourea, 5 parts of phenanthroline, 7 parts of citric acid and 15 parts of thioglycollic acid.
Semi-quantitative detection is carried out by utilizing binary chromogenic test paper, and the result is 4.45 multiplied by 10 -4 ～8.90×10 -4 Between mol/L, the data obtained by ICP examination was 7.09X 10 -4 And the mol/L is consistent with the range of the result obtained after comparison with a colorimetric plate, and the colors displayed among the three groups of parallel samples are also the same, which indicates that the test paper has better accuracy.
Example 5: detection of Cd (II) concentration in smelting treatment wastewater 1
Step 1, preparing PAN/Dz binary color development type test paper.
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.003 percent, and the mass concentration of the Dz chloroform solution is 0.0055 percent; and soaking the circular test paper with the diameter of 6mm in the test paper, taking out the circular test paper after 60min, and drying the circular test paper in a 50 ℃ oven to obtain the binary color development test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing serial Cd (II) solutions with concentration gradient of 8.90X 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the test paper into the binary color-developing test paper prepared in the step (1), developing for 90s, sucking the residual Cd (II) solution with absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
In the step 3, the measured water sample is wastewater after primary treatment of a certain nonferrous metal smelting plant in Shaanxi province, the wastewater contains interference ions such as Zn (II), cu (II), ni (II), pb (II) and the like, a masking agent for eliminating the interference of coexisting ions is added into the water sample before the water sample is transferred, and the masking agent comprises the following raw materials in parts by mass: 2 parts of thiourea, 2 parts of phenanthroline, 2 parts of citric acid and 26 parts of thioglycolic acid.
The concentration of Cd (II) in the measured water sample is 4.45 multiplied by 10 by comparing with a standard colorimetric plate -5 ～8.90×10 -5 Between mol/L, the data obtained by ICP detection is 6.28 multiplied by 10 -5 And the mol/L is consistent with the range of the result obtained by comparing the color comparison sample with the color comparison sample, and the colors displayed among the parallel samples are also the same, which shows that the test paper has good accuracy and applicability.
Example 6: detection of Cd (II) concentration in smelting treatment wastewater 2
Step 1, preparing PAN/Dz binary color development type test paper.
Preparing a binary color developing agent by using 0.3/0.2 mass ratio of PAN and Dz solution, wherein the mass concentration of the PAN chloroform solution is 0.0075%, and the mass concentration of the Dz chloroform solution is 0.003%; and soaking the circular test paper with the diameter of 6mm in the test paper, taking out the circular test paper after 50min, and drying the circular test paper in a 60 ℃ oven to obtain the binary color development test paper.
Step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing serial Cd (II) solutions with concentration gradient of 8.90X 10 -7 ～8.90×10 - 4 mol·L -1 And (2) dropwise adding the reagent solution on the binary color-developing test paper prepared in the step (1), developing for 60s, sucking the residual Cd (II) solution by using absorbent paper, drying, inspecting and taking reaction fragments, and preparing a PAN/Dz binary color-developing test paper standard colorimetric plate.
In the step 3, the measured water sample is wastewater after primary treatment of a certain nonferrous metal smelting plant in Shaanxi province, the wastewater contains interference ions such as Zn (II), cu (II), ni (II), pb (II) and the like, a masking agent for eliminating the interference of coexisting ions is added into the water sample before the water sample is transferred, and the masking agent comprises the following raw materials in parts by mass: 4 parts of thiourea, 6 parts of phenanthroline, 8 parts of citric acid and 13 parts of thioglycolic acid.
By reacting withComparing with standard colorimetric plate, the concentration of Cd (II) in the tested water sample is 4.45X 10 -5 ～8.90×10 -5 Between mol/L, the data obtained by ICP detection is 8.63 multiplied by 10 -5 And the mol/L is consistent with the range of the result obtained by comparing the color comparison sample with the color comparison sample, and the colors displayed among the parallel samples are also the same, which shows that the test paper has good accuracy and applicability.
In conclusion, the binary color-developing test paper and the method for rapidly and semi-quantitatively detecting Cd (II) provided by the invention have a wider detection range of Cd (II), and can be used for detecting Cd (II) with a concentration of 8.90 × 10 -7 ～8.90×10 -4 Semi-quantitative detection of Cd (II) between mol/L is realized, and LOD is 8.90 multiplied by 10 -7 The mol/L, the developing and the inspecting time are both 60s, the consumed time is short, the accuracy, the stability and the applicability are better, the test paper is easy to prepare, and the operation is simple.
The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts based on the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (6)
1. A method for rapidly and semi-quantitatively detecting Cd (II) by using binary chromogenic test paper is characterized by comprising the following steps:
step 1, preparing PAN/Dz binary color-developing test paper
Mixing the PAN chloroform solution and the Dz chloroform solution according to the mass ratio of 0.3/0.2 to prepare a PAN/Dz chloroform solution binary color developing agent, soaking the test paper in the PAN/Dz chloroform solution binary color developing agent, taking out the test paper after a certain time, and drying the test paper to obtain a binary color developing test paper;
the test paper is medium-speed qualitative filter paper, is soaked in PAN/Dz chloroform solution for 30-60 min and then taken out, and is dried in an oven at 40-60 ℃;
the mass concentration of the PAN chloroform solution is 0.003 to 0.015 percent, and the mass concentration of the Dz chloroform solution is 0.0015 to 0.0075 percent;
step 2, preparing a PAN/Dz binary color development type test paper standard colorimetric plate
Preparing a series of concentration gradient Cd (II) solutions, dropwise adding the solutions on the binary color-developing test paper prepared in the step (1), developing for a certain time, sucking the residual Cd (II) solutions by using absorbent paper, drying, inspecting and taking reaction fragments to prepare a PAN/Dz binary color-developing test paper standard colorimetric plate;
step 3, detecting Cd (II) solution with unknown concentration
And (3) adjusting the pH value of the Cd (II) solution to be detected, respectively adding a masking agent, dropwise adding the Cd (II) solution to be detected onto the binary color-developing test paper prepared in the step (1), detecting the color change, comparing the color change with the standard colorimetric plate prepared in the step (2), and carrying out semi-quantitative determination on the concentration of the Cd (II) solution to be detected.
2. The method for rapidly and semi-quantitatively detecting Cd (II) by using the binary chromogenic test paper as claimed in claim 1, wherein in the step 2, the chromogenic time is 30-90 s.
3. The method for quickly and semi-quantitatively detecting Cd (II) by using the binary color test paper as claimed in claim 1, wherein in step 3, the pH of a solution of Cd (II) to be detected is adjusted to 5-8.
4. The method for rapidly and semi-quantitatively detecting Cd (II) by using the binary chromogenic test paper as claimed in claim 1, wherein in the step 2, the concentration range of the series Cd (II) standard solution is 8.90 x 10 -7 ～8.90×10 -4 mol·L -1 。
5. The method for rapidly and semi-quantitatively detecting Cd (II) by using the binary chromogenic test paper as claimed in claim 1, wherein in the step 3, the masking agent comprises the following raw materials in parts by mass:
2-6 parts of thiourea, 2-6 parts of phenanthroline, 2-9 parts of citric acid and 13-26 parts of thioglycolic acid.
6. A test paper for binary color development used in accordance with any one of claims 1 to 5, wherein the test paper is obtained by immersing medium-speed quantitative filter paper in 0.003 to 0.015% PAN and 0.0015 to 0.0075% dz chloroform solution at a ratio of 0.3/0.2 for 30 to 60 minutes and drying the immersed paper in an oven at 40 to 60 ℃.
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