Beryllium element detection test paper as well as preparation method, detection method and application thereof

Abstract

The invention discloses beryllium element detection test paper as well as a preparation method, a detection method and application thereof. The beryllium element detection test paper comprises a filter paper base material, a color developing agent chrome azurol S and a shielding agent ethylene diamine tetraacetic acid disodium salt, the color developing agent chrome azurol S and the shielding agent disodium ethylene diamine tetraacetate are loaded on the filter paper base material. When the beryllium element detection test paper is used for detecting a surface beryllium pollution detection object, the detection method is simple and rapid to operate, high in sensitivity and low in cost.

Description

Technical Field

[0001] The invention relates to a beryllium element detection test paper and a preparation method, a detection method and an application thereof. Background Art

[0002] Beryllium is a lightweight, corrosion-resistant metal that is widely used in aerospace, nuclear industry and other fields. Beryllium particles mainly enter the human body through the respiratory tract and are slowly metabolized in the human body. Short-term exposure to high-concentration beryllium can cause acute beryllium poisoning, and long-term exposure to low-concentration beryllium can cause chronic beryllium disease. Existing studies have shown that fine particles can penetrate the skin and cause allergies. In 2017, the International Agency for Research on Cancer (IARC) classified beryllium as a Class 1 carcinogen. The Chronic Beryllium Disease Prevention and Control Plan issued by the U.S. Department of Energy (DOE) stipulates that the beryllium contamination limits for equipment and building surfaces in beryllium-involved and non-beryllium-involved workplaces are 3μg / 100cm 2 and 0.2 μg / 100 cm 2 . Therefore, the objects of environmental monitoring of beryllium pollution should include equipment and building surfaces that may be contaminated by beryllium. At present, the surface beryllium contamination monitoring method usually refers to the pre-treatment and analysis methods published by the Occupational Safety and Health Administration (OSHA) and the National Institute of Occupational Health (NIOSH) and other institutions in the United States. Beryllium on the contaminated surface is collected by wiping paper, and the wiping paper is digested and quantified by inductively coupled plasma mass spectrometry (ICP-MS). This method has high analysis costs and requires at least 24 hours to obtain analysis results.

[0003] Therefore, it is necessary to develop a simple, rapid technology that can detect the concentration of beryllium at the monitoring limit level. Summary of the invention

[0004] The technical problem to be solved by the present invention is to overcome the defects of the prior art in that the detection method of beryllium content on contaminated surfaces is time-consuming and costly, and to provide a beryllium element detection test paper and its preparation method, detection method, and application. When the beryllium element detection test paper of the present invention is used to detect beryllium-contaminated objects, the detection method is simple to operate, low in cost, and short in time.

[0005] The present invention adopts the following technical solutions to solve the above technical problems.

[0006] The present invention provides a beryllium element detection test paper, which comprises a filter paper substrate, a color developer chrome azuro blue S and a shielding agent disodium ethylenediaminetetraacetate;

[0007] The color developer chrome azuro blue S and the shielding agent disodium ethylenediaminetetraacetate are loaded on the filter paper substrate.

[0008] In the present invention, the selection of the filter paper substrate is extremely important for reducing the detection limit of the beryllium element detection test paper, because the properties of the filter paper substrate determine the amount of the color developer chrome azuro blue S and the shielding agent disodium ethylenediaminetetraacetate that can be loaded on it, and the content of the color developer chrome azuro blue S and the shielding agent disodium ethylenediaminetetraacetate, especially the content of the color developer chrome azuro blue S, is closely related to the detection limit of the beryllium element.

[0009] In the present invention, the filter paper substrate may be a Whatman Grade 1 filter paper, preferably Whatman Grade 1 with a diameter of 1-3 cm, more preferably Whatman Grade.1 with a diameter of 2.5 cm, such as Whatman Grade 11001-325 or Whatman Grade 1 1001-025.

[0010] In the present invention, the shielding agent disodium ethylenediaminetetraacetate can prevent interference from other metal ions except beryllium ions. The types of the other metal ions can be one or more of Al, Fe, Ni, Pb, Mg, Cu and Cr.

[0011] The present invention also provides a method for preparing a beryllium element detection test paper, which comprises the following steps:

[0012] S1, immersing the filter paper substrate in a color developer chrome azuro blue S solution, removing the solvent, and obtaining a first test paper;

[0013] S2. Immerse the first test paper in a shielding agent disodium ethylenediaminetetraacetic acid solution, remove the solvent, and obtain the test paper.

[0014] In the present invention, the filter paper substrate may be a Whatman Grade 1 filter paper, preferably Whatman Grade 1 with a diameter of 1-3 cm, more preferably Whatman Grade.1 with a diameter of 2.5 cm, such as Whatman Grade 11001-325 or Whatman Grade 1 1001-025.

[0015] In the present invention, the mass concentration of the developer chrome azure S solution can be conventional in the art, preferably 1%-10%, such as 1%, 5% or 8%. The mass concentration represents the percentage of the mass of the developer chrome azure S in the developer chrome azure S solution to the mass of the developer chrome azure S solution.

[0016] In a preferred embodiment, the mass concentration of the color developer chrome azure S solution is 1%, and the preparation method comprises: weighing 1 g of chrome azure S into a 100 ml volumetric flask, and making up to volume with ultrapure water.

[0017] In the present invention, the mass concentration of the shielding agent disodium ethylenediaminetetraacetate solution can be conventional in the art, preferably 1%-10%, such as 5% or 8%. The mass concentration represents the percentage of the mass of the shielding agent disodium ethylenediaminetetraacetate in the shielding agent solution to the mass of the shielding agent.

[0018] In a preferred embodiment, the mass concentration of the shielding agent disodium ethylenediaminetetraacetate solution is 5%, and the preparation method comprises: weighing 5 g of disodium ethylenediaminetetraacetate into a 100 ml volumetric flask, and making up to volume with ultrapure water.

[0019] In S1 of the present invention, the end point of the immersion may be a state where the filter paper substrate is saturated in the solution of the color developer chrome azuro blue S. The saturation means that the filter paper substrate will not absorb the color developer chrome azuro blue S solution even if the immersion time of the filter paper substrate is further extended.

[0020] In S1 of the present invention, the method for removing the solvent can be conventional in the art, preferably comprising immersing the filter paper substrate in a color developer chrome blue S solution, transferring it between two filter papers with a diameter larger than the filter paper substrate to press and remove excess color developer chrome blue S solution, and then drying it naturally.

[0021] In S2 of the present invention, the end point of the immersion may be a state where the first test paper is saturated in the shielding agent disodium ethylenediaminetetraacetic acid solution. The saturation means that if the immersion time of the first test paper is further extended, the first test paper will not absorb the shielding agent disodium ethylenediaminetetraacetic acid solution.

[0022] In S2 of the present invention, the method for removing the solvent may be conventional in the art, preferably comprising immersing the first test paper in a shielding agent disodium ethylenediaminetetraacetic acid solution, transferring the first test paper between two filter papers having a diameter larger than that of the first test paper, pressing to remove excess shielding agent disodium ethylenediaminetetraacetic acid solution, and then drying naturally.

[0023] The present invention also provides a beryllium element detection test paper, which is prepared by the preparation method of the beryllium element detection test paper as described above.

[0024] The present invention also provides a method for detecting beryllium, which comprises the following steps:

[0025] Wetting, sampling, coloring and comparing with the standard colorimetric card with the beryllium element detection test paper as described above;

[0026] The preparation method of the standard colorimetric card comprises the following steps: immersing the beryllium element detection test paper as described above in at least two beryllium solutions of different mass concentrations, developing color, preparing standard color blocks according to the color development results, and arranging the standard color blocks in sequence according to the concentration of the beryllium solution to prepare a standard colorimetric card;

[0027] The color development conditions in the beryllium detection method and the standard colorimetric card preparation method are consistent.

[0028] In the present invention, the wetting method may be conventional in the art, such as wetting with an ammonia solution.

[0029] The volume concentration of the ammonia solution may be 1%-10%, for example 5%.

[0030] In a preferred embodiment, the wetting step includes: spraying an ammonia solution with a volume concentration of 5% onto the beryllium detection test paper, and transferring it between two sheets of beryllium detection test paper with a diameter larger than that of the beryllium detection test paper to press and remove excess ammonia solution.

[0031] In the present invention, the sampling method can be conventional in the art, and preferably includes the following steps: pressing the moistened beryllium element detection test paper on the sampling surface, and slowly wiping the sampling surface.

[0032] The surface area of ​​the sample is preferably 100 cm 2 .

[0033] Among them, the sampling method preferably includes: sampling from top to bottom in a "Z" shape, the wiping process should cover the entire sampling surface, and / or, sampling from left to right in a "Z" shape, perpendicular to the previous wiping movement direction.

[0034] In the present invention, the color development can be performed by adjusting the pH of the wetted beryllium detection test paper to a pH at which color development can occur, preferably adjusting the pH of the beryllium detection test paper to 10. The method of adjusting the pH of the beryllium detection test paper to 10 can be conventional in the art, preferably including: spraying 0.1 ml of ammonia-ammonium chloride buffer solution with a pH of 10 on the beryllium detection test paper.

[0035] In the present invention, the beryllium solutions of different mass concentrations are preferably 5 different concentration gradients, such as 0 μg / mL, 2 μg / mL, 10 μg / mL, 30 μg / mL and 100 μg / mL.

[0036] In a preferred embodiment, the preparation method of the standard colorimetric card is: 0.1 ml of beryllium solution with a mass concentration of 0 μg / mL, 2 μg / mL, 10 μg / mL, 30 μg / mL, and 100 μg / mL is added to the beryllium element detection test paper, and then 0.1 ml of ammonia-ammonium chloride buffer solution is sprayed on the test paper to adjust the pH of the test paper to 10. After the color reaction occurs for 1-3 minutes, the color is taken using a colorimeter to prepare a standard colorimetric card.

[0037] The present invention also provides an application of the above-mentioned beryllium element detection method in the field of beryllium pollution detection.

[0038] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0039] The reagents and raw materials used in the present invention are commercially available.

[0040] The positive and progressive effects of the present invention are:

[0041] (1) In the present invention, the color developer chrome azuro blue S and the shielding agent disodium ethylenediaminetetraacetate are loaded on a filter paper substrate to obtain a beryllium element detection test paper. In the test paper, the shielding agent disodium ethylenediaminetetraacetate can combine with the interfering metal ions that may exist on the sampling surface to prevent the interfering metal ions from occupying the complexing sites of chrome azuro blue S, ensuring that the color developer chrome azuro blue S is complexed with beryllium ions to generate blue complex molecules to achieve qualitative or semi-quantitative detection of beryllium ions on the contaminated surface.

[0042] (2) The beryllium element detection test paper prepared by the present invention is sensitive and rapid, and the detection limit for the surface beryllium contamination level is 0.2 μg / 100 cm 2 , meeting the monitoring limit requirements.

[0043] (3) The beryllium detection method of the present invention is simple to operate, short in time and low in cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 This is the color development result of the test paper after adding different masses of beryllium ions.

[0045] Figure 2 The standard colorimetric card is prepared.

[0046] Figure 3 Part a is the color development result of the beryllium element detection paper after adding 0.1ml of interfering metal ion solution with a mass concentration of 100μg / mL; Figure 3 Part b is the color development result of the beryllium element detection test paper after adding 0.1 ml of 100 μg / mL interfering metal ion solution and 0.1 ml of 10 μg / mL beryllium solution. DETAILED DESCRIPTION

[0047] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods in the following examples without specifying specific conditions are carried out according to conventional methods and conditions, or selected according to the product specifications.

[0048] Example 1

[0049] Preparation of Beryllium Test Paper:

[0050] S1. Select Whatman Grade.1 standard qualitative filter paper (model: Whatman Grade 11001-325) with a diameter of 2.5 cm as the filter paper substrate, immerse the filter paper substrate in a chromogenic agent chrome azuro blue S solution with a mass concentration of 1% until saturation (saturation means that the filter paper substrate cannot absorb more solution by continuing to extend the immersion time of the filter paper substrate, which is specifically manifested as the solution dripping from the filter paper substrate by continuing to extend the immersion time of the filter paper substrate), and transfer it between two filter papers with a diameter of 7 cm (Q5780 slow qualitative filter paper, purchased from Aladdin) and press to remove excess chromogenic agent chrome azuro blue S solution, and then dry it naturally in a fume hood to remove the solvent, to obtain the first test paper; wherein, the chromogenic agent chrome azuro blue S solution with a mass concentration of 1% is obtained by weighing 1 g of chrome azuro blue S into a 100 ml volumetric flask and making up to volume with ultrapure water;

[0051] S2. Immerse the first test paper in a shielding agent (disodium ethylenediaminetetraacetic acid) solution with a mass concentration of 5% until saturation (saturation means that the first test paper can no longer absorb more solution by continuing to extend the immersion time of the first test paper, which is specifically manifested as solution dripping from the first test paper by continuing to extend the immersion time of the first test paper), transfer it between two filter papers with a diameter of 7 cm and press to remove excess shielding agent solution, dry it naturally in a fume hood to remove the solvent, and obtain a beryllium element detection test paper; wherein, the disodium ethylenediaminetetraacetic acid solution with a mass concentration of 5% is obtained by weighing 5g of disodium ethylenediaminetetraacetic acid into a 100ml volumetric flask and making up to volume with ultrapure water.

[0052] Detection method of beryllium:

[0053] (1) Wetting: Spray 0.1 ml of 5% ammonia solution onto the beryllium test paper prepared above, transfer it between two filter papers with a diameter of 7 cm and press to remove excess ammonia solution;

[0054] (2) Sampling: Press the wetted test paper in step (1) onto the sampling surface (100 cm 2 The sample is taken from top to bottom in a "Z" shape, and the wiping process should cover the entire sampling surface. Then, the sample is taken from left to right in a "Z" shape, perpendicular to the previous wiping direction.

[0055] (3) Spray 0.1 ml of ammonia-ammonium chloride buffer solution with a pH of 10 on the test paper of step (2). After 1-3 minutes, observe the color of the test paper and compare it with a standard colorimetric card to detect the level of beryllium contamination on the surface based on the color and depth. The preparation method of the ammonia-ammonium chloride buffer solution with a pH of 10 is as follows: weigh 5.45 g of ammonium chloride and dissolve it in ultrapure water, add 35 ml of ammonia water, and dilute to a 100 ml volumetric flask.

[0056] Among them, the preparation method of the standard colorimetric card is: respectively drop 0.1 ml of beryllium solutions with mass concentrations of 0 μg / mL, 2 μg / mL, 10 μg / mL, 30 μg / mL, and 100 μg / mL (the above beryllium solutions with different mass concentrations are obtained by diluting the beryllium standard solution with model number B115394 and mass concentration of 1000 μg / mL purchased from Aladdin) on the beryllium element detection test paper prepared in S2, and then spray 0.1 ml of ammonia-ammonium chloride buffer solution with a pH of 10 onto the test paper. After the color reaction occurs for 1-3 minutes, use a colorimeter to take the color to make a standard colorimetric card.

[0057] The color development results of the test paper after adding different masses of beryllium ions are as follows Figure 1 As shown; among them, Figure 1 The a part is the color of the beryllium element detection test paper prepared above. Figure 1 Part b is the result of the color reaction of the test paper loaded with 0 μg beryllium ions. Figure 1 Part c is the result of the color reaction of the test paper loaded with 0.2 μg beryllium ions. Figure 1 Part d is the result of the color reaction of the test paper loaded with 1 μg of beryllium ions. Figure 1 Part e is the result of the color reaction of the test paper loaded with 3μg beryllium ions. Figure 1 Part f shows the result of the color reaction of the test paper loaded with 10 μg of beryllium ions.

[0058] in accordance with Figure 1 The standard color chart made of Figure 2 As shown, Figure 2 The a part is the color presented by the beryllium element detection test paper prepared above. Figure 2 Part b is the color of the test paper loaded with 0 μg beryllium ions after color development. Figure 2 Part c is the color of the test paper loaded with 0.2 μg beryllium ions after color development. Figure 2 Part d is the color of the test paper loaded with 1 μg beryllium ions after color development. Figure 2 Part e is the color of the test paper loaded with 3 μg beryllium ions after color development. Figure 2 Part f shows the color of the test paper loaded with 10 μg of beryllium ions.

[0059] Example 2

[0060] 0.1 ml of the interfering ion solution with a mass concentration of 100 μg / mL (the above solution is obtained by diluting the standard solution with a model number of BWB2259 and a concentration of 1000 μg / mL purchased from Weiye Metrology Institute) is added to the beryllium element detection test paper prepared in Example 1, and 0.1 ml of ammonia-ammonium chloride buffer solution is sprayed on the test paper. After 1-3 minutes, the color of the test paper is observed. The results are as follows: Figure 3As shown in part a of the figure. Add 0.1 ml of interfering ion solution with a mass concentration of 100 μg / mL, then add 0.1 ml of beryllium solution with a mass concentration of 10 μg / mL, and spray 0.1 ml of ammonia-ammonium chloride buffer solution on the test paper after sampling. After 1-3 minutes, observe the color of the test paper. The result is as follows: Figure 3 As shown in part b.

[0061] Depend on Figure 3 Comparing part a and part b, it can be seen that the shielding agent in the test paper can effectively combine with the interfering ions to prevent the interfering ions from occupying the complexing sites of the color developer chrome azuro blue S.

Claims

1. A beryllium element detection test paper, characterized in that: It includes filter paper substrate, color developing agent chrome azuro blue S and shielding agent disodium ethylenediaminetetraacetate; The color developer chrome azuro blue S and the shielding agent disodium ethylenediaminetetraacetate are loaded on the filter paper substrate.

2. The beryllium detection test paper according to claim 1, characterized in that: The filter paper substrate is a filter paper of the model Whatman Grade 1, preferably Whatman Grade 1 with a diameter of 1-3 cm, more preferably Whatman Grade.1 with a diameter of 2.5 cm, such as Whatman Grade 1 1001-325 or Whatman Grade 1 1001-025.

3. A method for preparing a beryllium element detection test paper, characterized in that: It includes the following steps: S1, immersing the filter paper substrate in a color developer chrome azuro blue S solution, removing the solvent, and obtaining a first test paper; S2. Immerse the first test paper in a shielding agent disodium ethylenediaminetetraacetic acid solution, remove the solvent, and obtain the test paper.

4. The method for preparing the beryllium element detection test paper according to claim 3, wherein: The filter paper substrate is a Whatman Grade 1 filter paper, preferably Whatman Grade 1 with a diameter of 1-3 cm, more preferably Whatman Grade 1 with a diameter of 2.5 cm, such as Whatman Grade 1 1001-325 or Whatman Grade 1 1001-025.

5. The method for preparing the beryllium element detection test paper according to claim 3, characterized in that: The preparation method of the beryllium element detection test paper meets one or more of the following conditions: (1) The mass concentration of the developer chrome azuro blue S solution is 1%-10%, for example, 1%, 5% or 8%; (2) The mass concentration of the shielding agent disodium ethylenediaminetetraacetic acid solution is 1%-10%, for example, 5% or 8%; (3) In S1, the end point of the immersion is when the filter paper substrate is saturated in the chromogenic agent chrome azuro blue S solution; the saturation means that the filter paper substrate will not absorb the chromogenic agent chrome azuro blue S solution even if the immersion time of the filter paper substrate is further extended; (4) In S1, the method for removing the solvent comprises immersing the filter paper substrate in a color developer chrome azuro blue S solution, transferring the filter paper substrate between two filter papers having a diameter larger than the filter paper substrate, pressing to remove excess color developer chrome azuro blue S solution, and then drying the filter paper substrate naturally; (5) In S2, the end point of the immersion is when the first test paper is saturated in the shielding agent disodium ethylenediaminetetraacetic acid solution; the saturation means that if the immersion time of the first test paper is further extended, the first test paper will not absorb the shielding agent disodium ethylenediaminetetraacetic acid solution; (6) In S2, the method for removing the solvent comprises immersing the first test paper in a shielding agent disodium ethylenediaminetetraacetic acid solution, transferring the first test paper between two filter papers having a diameter larger than that of the first test paper, pressing to remove excess shielding agent disodium ethylenediaminetetraacetic acid solution, and then drying naturally.

6. A beryllium element detection test paper, characterized in that: The beryllium element detection test paper is prepared by the preparation method of the beryllium element detection test paper as described in any one of claims 3 to 5.

7. A method for detecting beryllium, characterized in that: It includes the following steps: Wetting, sampling, coloring, and comparing with a standard colorimetric card according to any one of claims 1 to 2 and claim 6; The preparation method of the standard colorimetric card comprises the following steps: immersing the beryllium element detection test paper according to any one of claims 1 to 2 and claim 6 in at least two beryllium solutions of different mass concentrations, developing color, preparing standard color blocks according to the color development results, and arranging the standard color blocks in sequence according to the concentration of the beryllium solution to prepare a standard colorimetric card; The color development conditions in the beryllium detection method and the standard colorimetric card preparation method are consistent.

8. The method for detecting beryllium according to claim 7, characterized in that: The beryllium detection method meets one or more of the following conditions: (1) The wetting is performed by wetting with an ammonia solution; (2) The sampling method includes the following steps: pressing the moistened beryllium element detection paper onto the sampling surface and slowly wiping the sampling surface; (3) The color development is performed by adjusting the pH of the wetted beryllium detection test paper to a pH at which color development can occur, preferably adjusting the pH of the beryllium detection test paper to 10; (4) The beryllium solutions of different mass concentrations are preferably 5 different concentration gradients, such as 0 μg / mL, 2 μg / mL, 10 μg / mL, 30 μg / mL and 100 μg / mL.

9. The method for detecting beryllium as claimed in claim 8, characterized in that: The beryllium detection method meets one or more of the following conditions: (1) The volume concentration of the ammonia solution is 1%-10%, for example 5%; (2) The surface area of ​​the sample is 100 cm 2 ; (3) The sampling methods include: sampling from top to bottom in a "Z" shape, the wiping process should cover the entire sampling surface, and / or, sampling from left to right in a "Z" shape, perpendicular to the direction of the previous wiping movement; (4) The method of adjusting the pH of the beryllium detection test paper to 10 includes: spraying 0.1 ml of ammonia-ammonium chloride buffer solution with a pH of 10 on the beryllium detection test paper.

10. Application of the beryllium detection method according to any one of claims 7 to 9 in the field of beryllium pollution detection.

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