Digestion method for detecting all elements of high-purity metal sodium

Abstract

The invention discloses a digestion method for all-element detection of high-purity metallic sodium, and belongs to the technical field of detection methods, and the digestion method comprises the following steps: S1, placing a container filled with metallic sodium in an inert gas environment; s2, injecting more than 0.1 ml of purified water, deionized water, ultrapure water, diluted hydrochloric acid or diluted sulfuric acid into the container, reacting with the metal sodium, standing for 1-5 minutes, and repeating the step until the metal sodium is completely dissolved; s3, injecting purified water, deionized water, ultrapure water, diluted hydrochloric acid or diluted sulfuric acid into the container, and uniformly stirring to obtain the digestion solution. The digestion method provided by the invention not only avoids the combustion and explosion risks of direct detection of the metal sodium, but also avoids the pollution of oxides to the detected product during direct detection of the metal sodium, thereby improving the detection precision of the metal sodium component.

Description

Technical Field

[0001] The invention belongs to the technical field of detection methods, and in particular relates to a digestion method for full-element detection of high-purity metallic sodium. Background Art

[0002] With the continuous development of the sodium metal application market, sodium metal is increasingly widely used. At the same time, the composition detection and analysis of high-purity sodium is a prerequisite for industry use, and the detection work is becoming more and more frequent. However, sodium metal products are extremely active and will be oxidized when in contact with air. They are particularly dangerous for combustion and explosion, which brings great troubles to the detection work. Therefore, it is extremely necessary to digest them scientifically and safely.

[0003] The test products generally provided must be easy to detect and ensure that their original components are not disturbed, which poses new major challenges to the digestion work. At present, the common digestion methods generally use concentrated acid, aqua regia, liquid ammonia and other dangerous chemicals for digestion, which have the disadvantages of dangerous operation, difficult implementation and extremely high cost.

[0004] In view of the fact that currently no major testing institutions have proposed a relatively reasonable and scientific digestion method, there is an urgent need for a digestion method that can make the digestion and detection of metallic sodium extremely convenient. Summary of the invention

[0005] The purpose of the present invention is to provide a digestion method for full-element detection of high-purity metallic sodium, which is more scientific, safe and convenient, thereby making the digestion detection of metallic sodium extremely convenient.

[0006] To achieve the purpose of the present invention, the technical solution adopted is: a digestion method for full-element detection of high-purity metallic sodium, comprising the following steps:

[0007] S1. Place a container containing metallic sodium in an inert gas environment;

[0008] S2. Inject more than 0.1 ml of one of pure water, deionized water, ultrapure water, dilute hydrochloric acid, and dilute sulfuric acid into the container as an intermediate, and let it stand for 1 to 5 minutes after reacting with metallic sodium. Repeat this step until the metallic sodium is completely dissolved; wherein the ratio of metallic sodium to the intermediate is 1:1 to 1:10.

[0009] S3. Inject one of pure water, deionized water, ultrapure water, dilute hydrochloric acid, and dilute sulfuric acid into the container as an intermediate, and stir evenly to obtain a digestion solution; wherein the ratio of metallic sodium to the intermediate is 1:1 to 1:100.

[0010] Furthermore, the container containing metallic sodium in step S1 is sealed before being placed in the inert gas environment.

[0011] Furthermore, in step S1, the amount of metallic sodium in the container is 1-2 ml.

[0012] Furthermore, the container containing metallic sodium in step S1 is a 2-5 ml vial.

[0013] Furthermore, the inert gas environment in step S1 is an inert gas glove box.

[0014] Furthermore, in step S2, the device for injecting pure water, deionized water, ultrapure water, dilute hydrochloric acid or dilute sulfuric acid into the container is a micro plastic syringe.

[0015] Furthermore, the container in step S3 is a 250 ml crimp-top glass bottle.

[0016] Furthermore, in step S3, the device for injecting pure water, deionized water, ultrapure water, dilute hydrochloric acid or dilute sulfuric acid into the container is a 50 ml plastic syringe.

[0017] Furthermore, the stirring tool in step S3 is a stirring rod made of an inert material.

[0018] Furthermore, the digestion solution obtained in step S3 is 100 ml.

[0019] In the present invention, the ratio of metallic sodium to the intermediate can be adjusted according to the mass of metallic sodium. When the mass of metallic sodium changes, the digestion method of metallic sodium is not adjusted, and only the ratio of metallic sodium to the intermediate is adjusted.

[0020] The beneficial effects of the present invention are:

[0021] The digestion method provided by the present invention not only avoids the combustion and explosion risks of direct detection of metallic sodium, but also avoids the contamination of the detection product by oxides that appear when directly detecting metallic sodium, thereby improving the accuracy of metallic sodium component detection; at the same time, the digestion method provided by the present invention has the advantages of extremely low implementation cost, fast and efficient, safe and environmentally friendly, and is particularly conducive to scientific and accurate detection. DETAILED DESCRIPTION

[0022] Example 1

[0023] The present embodiment provides a digestion method for full-element detection of high-purity metallic sodium, comprising the following steps:

[0024] S1. Place 1-2 ml of metallic sodium in a 2-5 ml vial and seal the mouth of the vial.

[0025] S2. Place a vial containing metallic sodium, a 250 ml crimp glass bottle, a 1 ml plastic syringe, a 50 ml plastic syringe, and a 30 cm long glass stirring rod in an inert gas glove box, and place 500 ml of pure water in the inert gas glove box. The oxygen content in the inert gas glove box is ≤1 ppm, and the humidity in the inert gas glove box is ≤0.1% RH.

[0026] S3. Put both hands into the gloves in the inert gas glove box, open the mouth of the vial containing metallic sodium, draw 1 ml of pure water with a 1 ml plastic syringe, initially inject more than 0.1 ml of pure water into the vial, and the injection rate of pure water is 5 μL / s. After the pure water reacts with the metallic sodium, let it stand for 1 minute, inject 0.1 ml of pure water into the vial again, and continue to let it stand for 1 minute. Repeat this step until the pure water in the syringe is dripped and the metallic sodium is completely dissolved;

[0027] S4. Use a 1 ml plastic syringe to transfer all the dissolved solution in the vial into a 250 ml crimp-top glass bottle;

[0028] S5. Use a 50 ml plastic syringe to draw 50 ml of pure water and slowly inject it into the clamp-top glass bottle, then stir with a 30 cm glass stirring rod. Repeat this step until the solution in the clamp-top glass bottle reaches 100 ml, and use a 30 cm glass stirring rod to stir evenly to obtain a digestion solution.

[0029] S6. Seal the crimp-top glass bottle and the digestion work is completed; or use a 50ml plastic syringe to dispense the digestion solution in the crimp-top glass bottle as needed.

[0030] The recovery rate of metallic sodium was 99.2-101.8% and RSD<0.5% as detected by ICP-MS.

[0031] Example 2

[0032] The present embodiment provides a digestion method for full-element detection of high-purity metallic sodium, comprising the following steps:

[0033] S1. Place 1-2 ml of metallic sodium in a 2-5 ml vial and seal the mouth of the vial.

[0034] S2. Place a vial containing metallic sodium, a 250 ml crimp glass bottle, a 1 ml plastic syringe, a 50 ml plastic syringe, and a 30 cm long glass stirring rod in an inert gas glove box, and place 500 ml of dilute hydrochloric acid in the inert gas glove box. The oxygen content in the inert gas glove box is ≤1 ppm, and the humidity in the inert gas glove box is ≤0.1% RH.

[0035] S3. Put both hands into the gloves in the inert gas glove box, open the mouth of the vial containing metallic sodium, draw 1 ml of dilute hydrochloric acid with a 1 ml plastic syringe, initially inject more than 0.1 ml of dilute hydrochloric acid into the vial, and the injection rate of dilute hydrochloric acid is 5 μL / s. After the dilute hydrochloric acid reacts with the metallic sodium, let it stand for 1 minute, inject 0.1 ml of dilute hydrochloric acid into the vial again, and continue to let it stand for 1 minute. Repeat this step until the pure dripping in the syringe is completed and the metallic sodium is completely dissolved;

[0036] S4. Use a 1 ml plastic syringe to transfer all the dissolved solution in the vial into a 250 ml crimp-top glass bottle;

[0037] S5. Use a 50 ml plastic syringe to draw 50 ml of dilute hydrochloric acid and slowly inject it into the clamp-top glass bottle, then stir with a 30 cm glass stirring rod. Repeat this step until the solution in the clamp-top glass bottle reaches 100 ml, and use a 30 cm glass stirring rod to stir evenly to obtain a digestion solution.

[0038] S6. Seal the crimp-top glass bottle and the digestion work is completed; or use a 50ml plastic syringe to dispense the digestion solution in the crimp-top glass bottle as needed.

[0039] The recovery rate of metallic sodium was 99.2-101.8% and RSD<0.5% as detected by ICP-MS.

[0040] It should be understood by those skilled in the art that the above embodiments are only for the purpose of clearly illustrating the present invention, and are not intended to limit the scope of the present invention. For those skilled in the art, other changes or modifications may be made based on the above disclosure, and these changes or modifications are still within the scope of the present invention.

Claims

1. A digestion method for full element detection of high-purity metallic sodium, characterized in that: The steps include: S1. Place a container containing metallic sodium in an inert gas environment; S2. Inject more than 0.1 ml of one of pure water, deionized water, ultrapure water, dilute hydrochloric acid, and dilute sulfuric acid into the container as an intermediate, and let it stand for 1 to 5 minutes after reacting with metallic sodium, and repeat this step until the metallic sodium is completely dissolved; wherein the ratio of metallic sodium to the intermediate is 1:1 to 1:10; S3. Inject one of pure water, deionized water, ultrapure water, dilute hydrochloric acid, and dilute sulfuric acid into the container as an intermediate, and stir evenly to obtain a digestion solution; wherein the ratio of metallic sodium to the intermediate is 1:1 to 1:

100.

2. The digestion method for full element detection of high-purity metallic sodium according to claim 1, characterized in that: The container containing metallic sodium in step S1 is sealed before being placed in an inert gas environment.

3. The digestion method for full element detection of high-purity metallic sodium according to claim 1, characterized in that: In step S1, the amount of metallic sodium in the container is 1-2 ml.

4. The digestion method for full element detection of high-purity metallic sodium according to claim 1, characterized in that: The container containing metallic sodium in step S1 is a 2-5 ml vial.

5. The digestion method for full element detection of high-purity metallic sodium according to claim 1, characterized in that: The inert gas environment in step S1 is an inert gas glove box.

6. The digestion method for full element detection of high-purity metallic sodium according to any one of claims 1 to 5, characterized in that: In step S2, the device for injecting pure water, deionized water, ultrapure water, dilute hydrochloric acid or dilute sulfuric acid into the container is a micro plastic syringe.

7. The digestion method for full element detection of high-purity metallic sodium according to any one of claims 1 to 5, characterized in that: The container in step S3 is a 250 ml crimp-top glass bottle.

8. The digestion method for full element detection of high-purity metallic sodium according to any one of claims 1 to 5, characterized in that: In step S3, the device for injecting pure water, deionized water, ultrapure water, dilute hydrochloric acid or dilute sulfuric acid into the container is a 50 ml plastic syringe.

9. The digestion method for full element detection of high-purity metallic sodium according to any one of claims 1 to 5, characterized in that: The stirring tool in step S3 is a stirring rod made of an inert material.

10. The digestion method for full element detection of high-purity metallic sodium according to any one of claims 1 to 5, characterized in that: The digestion solution obtained in step S3 is 100 ml.