Dry storage box for samples easy to absorb moisture and method for testing oxygen content of samples

Abstract

The invention discloses an easy-moisture-absorption sample drying storage box and a sample oxygen content testing method, the easy-moisture-absorption sample drying storage box comprises a box body, a rotating disc, a sample container and a drying agent, an inner cavity is arranged in the box body, one side of the box body is provided with an opening communicated with the inner cavity, and the rotating disc is pivoted in the box body through a pivot shaft; the pivoting shaft is parallel to the central axis of the box body and deviates from the central axis of the box body; at least two accommodating grooves are concavely formed in the upper surface of the turntable, and the sample containers are respectively accommodated in the accommodating grooves; the box body is provided with an interlayer above the inner cavity, and the drying agent is arranged in the interlayer; an air hole communicated with the inner cavity is formed in the bottom of the interlayer, an annular sealing ring is arranged at the bottom of the interlayer, and the sealing ring surrounds the periphery of the air hole. The device is good in sealing performance, effectively prevents a sample from getting damp in the process of waiting for testing, improves the measurement accuracy, and is convenient to use.

Description

Technical Field

[0001] The invention relates to the technical field of battery material testing, and in particular to a drying storage box for moisture-absorbing samples and a method for testing the oxygen content of the samples. Background Art

[0002] In the process of battery material production, it is often necessary to test the oxygen content of battery materials. Taking coke as an example, in order to test the oxygen content of coke, it is necessary to take out a certain mass of coke sample and place it on a high-frequency infrared oxygen and nitrogen instrument for measurement. In addition, in order to ensure the accuracy of the measurement, it is necessary to take out multiple samples and measure them multiple times, and then take the average value. However, while these samples are waiting in line for testing, the untested samples are exposed to moisture and are easily exposed to moisture, which leads to unstable and high oxygen content data of the sample test, resulting in inaccurate measurement data of the sample, affecting the performance of the finished battery. Summary of the invention

[0003] The purpose of the present invention is to provide a moisture-absorbing sample drying storage box which has good sealing performance, effectively prevents the sample from absorbing moisture while waiting for testing, improves the accuracy of the measurement, and is easy to use.

[0004] Another object of the present invention is to provide a method for testing the oxygen content of a hygroscopic sample, which can prevent the sample from dehumidifying while waiting for testing and has high measurement accuracy.

[0005] In order to achieve the above-mentioned purpose, the present invention provides a drying and storage box for hygroscopic samples, comprising a box body, a turntable, a sample container and a desiccant, wherein an inner cavity is arranged in the box body, an opening communicating with the inner cavity is arranged on one side of the box body, and the turntable is pivotally connected to the box body through a pivot axis, so that the turntable can be rotated into or out of the inner cavity through the opening; the pivot axis is parallel to the central axis of the box body and deviates from the central axis of the box body; at least two accommodating grooves are formed in a concave manner on the upper surface of the turntable, and the sample containers are respectively accommodated in the accommodating grooves; the box body is provided with a partition layer above the inner cavity, and the desiccant is arranged in the partition layer; an air vent communicating with the inner cavity is formed at the bottom of the partition layer, and an annular sealing ring is provided at the bottom of the partition layer, and the sealing ring surrounds the outer periphery of the air vent, and when the turntable is located in the inner cavity, the sealing ring is in sealing contact with the outer periphery of the upper surface of the turntable.

[0006] Compared with the prior art, the present invention provides a turntable in a rotatable manner in the box body, and at least two receiving grooves are provided in a concave manner on the upper surface of the turntable, so that the receiving grooves can be used to accommodate sample containers containing samples. Since the turntable can be rotated in or out of the box body, the sample can be sent in or out of the turntable through the turntable, so as to achieve the purpose of quickly testing the sample, and it is very convenient to use. In addition, since a partition layer connected to the inner cavity is provided above the inner cavity of the box body, a desiccant is provided in the partition layer, and a sealing ring in sealing contact with the turntable is provided at the bottom of the partition layer, when the sample is sent into the turntable, the sample can be isolated from the outside world, and the desiccant can dry the sample, so as to effectively prevent the sample from dehumidifying while waiting for the test, and greatly improve the accuracy of the test.

[0007] Preferably, a cover body is provided on the upper side of the box body, which can open or seal the interlayer, so that the desiccant in the interlayer can be quickly replaced, thereby improving the convenience of use.

[0008] Preferably, a buffer pad is provided around the opening, and when the rotating disk rotates into or out of the inner cavity, the outer wall of the rotating disk slides in contact with the buffer pad. The buffer pad can increase the friction between the two when the rotating disk rotates into or out of the box body, preventing the sample from flying out due to the rotating disk rotating too fast, and also ensures a certain waterproof sealing performance between the rotating box and the box body.

[0009] Preferably, the pivot axis is located on the outer circumference of the box body. By moving the pivot axis away from the central axis of the box body, the turntable can be rotated out of the box body at a large angle, so that more samples can be placed on the turntable, thereby increasing the sample capacity of the storage box.

[0010] Preferably, the box body is a cylindrical structure, and the turntable is a cylindrical structure.

[0011] Preferably, the sample container is a nickel crucible.

[0012] Preferably, the upper surface of the turntable is concavely provided with at least two access openings symmetrically arranged on both sides of the receiving groove, and one side of the access opening is connected to the receiving groove. The access opening can be entered by a finger or a tool, so as to facilitate the sample container to be clamped from the receiving groove, thereby improving the convenience of taking and placing the sample container.

[0013] A method for testing the oxygen content of a hygroscopic sample using a hygroscopic sample dry storage box comprises the following steps:

[0014] Open the sample bag and dry it in an oven;

[0015] Putting a certain mass of the dried sample into the sample container and recording it as the first sample;

[0016] placing the first sample into a high-frequency infrared oxygen and nitrogen instrument to measure the oxygen content of the first sample;

[0017] Put another dried sample of the same mass into another sample container and record it as the second sample;

[0018] During the measurement of the first sample, the second sample is placed in the receiving groove of the rotating disk, and then the rotating disk is closed to keep the second sample dry in the box body;

[0019] After the test of the first sample is completed, the second sample is taken out from the turntable and put into the high-frequency infrared oxygen and nitrogen analyzer to measure the oxygen content of the second sample.

[0020] Preferably, before placing the sample into the sample container, the empty sample container is first placed on a weighing device for taring.

[0021] Preferably, before placing the first sample into the high-frequency infrared oxygen and nitrogen analyzer, the first sample is placed in a receiving groove of the turntable to keep the first sample dry in the box body. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a three-dimensional view of the rotating disk of the sample drying storage box for measuring oxygen content of the present invention when it is closed.

[0023] Figure 2 The present invention is a state diagram of a sample drying and storage box for measuring oxygen content when the turntable is opened.

[0024] Figure 3 It is an internal cross-sectional view of a sample drying and storage box for measuring oxygen content of the present invention.

[0025] Figure 4 It is a flow chart of the method for testing the oxygen content of hygroscopic samples of the present invention. DETAILED DESCRIPTION

[0026] In order to explain the technical content, structural features and achieved effects of the present invention in detail, the following is a detailed description in conjunction with the implementation methods and the accompanying drawings.

[0027] like Figures 1 to 3As shown, the drying storage box 100 for hygroscopic samples of the present invention comprises a box body 1, a turntable 2, a sample container 3 and a desiccant 4. The box body 1 is provided with an inner cavity 11, and one side of the box body 1 is provided with an opening 12 connected to the inner cavity 11. The turntable 2 is pivoted in the box body 1 through a pivot shaft 21, so that the turntable 2 can be rotated into or out of the inner cavity 11 through the opening 12. The box body 1 is a cylindrical structure, and the turntable 2 is a cylindrical structure. The pivot shaft 21 is parallel to the central axis of the box body 1 and deviates from the central axis of the box body 1; in this embodiment, the pivot shaft 21 is located on the outer circumference of the box body 1. By moving the pivot shaft 21 away from the central axis of the box body 1, the turntable 2 can be rotated out of the box body 1 at a large angle, so that more samples can be placed on the turntable 2, thereby increasing the sample capacity of the storage box. When the turntable 2 is built into the box body 1, the central axis of the turntable 2 is coaxial with the central axis of the box body 1. The upper surface of the turntable 2 is concavely provided with at least two receiving grooves 22, and the sample containers 3 are respectively received in the receiving grooves 22; the sample containers 3 are nickel crucibles. In this embodiment, the outer diameter of the turntable 2 is 60 mm and the height is 17.5 mm; the diameter of the receiving groove 22 of the turntable 2 is 9 mm and the depth is 17 mm. The outer diameter of the sample container 3 is slightly smaller than 9 mm and the height is 17 mm, so that it can be just installed in the receiving groove 22. The box body 1 is provided with a partition 13 above the inner cavity 11, and the desiccant 4 is arranged in the partition 13; the desiccant 4 is silica gel, molecular sieve or other dehumidifying desiccant. The bottom of the interlayer 13 is provided with an air hole 131 communicating with the inner cavity 11, and the bottom of the interlayer 13 is provided with an annular sealing ring 132, which surrounds the outer periphery of the air hole 131. When the turntable 2 is located in the inner cavity 11, the sealing ring 132 is in sealing contact with the outer periphery of the upper surface of the turntable 2. The upper side of the box body 1 is provided with a cover 133 that can open or seal the interlayer 13. In this way, the desiccant 4 in the interlayer 13 can be quickly replaced, thereby improving the convenience of use.

[0028] For example Figure 2 and Figure 3 The upper surface of the turntable 2 is concavely provided with at least two access openings 23 symmetrically arranged on both sides of the receiving groove 22, and one side of the access opening 23 is connected with the receiving groove 22. The access opening 23 can be entered by a finger or a tool, so as to facilitate the sample container 3 to be clamped from the receiving groove 22, thereby improving the convenience of taking and placing the sample container 3.

[0029] See also Figure 1 and Figure 2, a cushion pad 14 is provided around the opening 12, and when the turntable 2 rotates into or out of the inner cavity 11, the outer wall of the turntable 2 slides in contact with the cushion pad 14. The cushion pad 14 is a cotton layer or any material with a cushioning and waterproof effect. Through the cushion pad 14, the friction between the two can be increased when the turntable 2 rotates into or out of the box body 1 to prevent the turntable 2 from rotating too fast and causing the sample to fly out, and a certain waterproof sealing performance can be achieved between the turntable box and the box body 1. The side wall of the turntable 2 exposed from the opening 12 is recessed with a card slot or friction protrusion 2a for the finger to apply force, so as to rotate the turntable 2 out of the box body 1.

[0030] Compared with the prior art, the present invention provides a rotating disk 2 in the box body 1, and at least two receiving grooves 22 are provided in a concave manner on the upper surface of the rotating disk 2, so that the receiving grooves 22 can be used to accommodate the sample container 3 containing the sample. Since the rotating disk 2 can be rotated in or out of the box body 1, the sample can be sent into or out of the rotating disk 2 through the rotating disk 2, so as to achieve the purpose of quickly testing the sample, and it is very convenient to use. In addition, since a partition 13 connected to the inner cavity 11 is provided above the inner cavity 11 of the box body 1, and a desiccant 4 is provided in the partition 13, and a sealing ring 132 in sealing contact with the rotating disk 2 is provided at the bottom of the partition 13, when the sample is sent into the rotating disk 2, the sample can be isolated from the outside world, and the desiccant 4 can dry the sample, so as to effectively prevent the sample from dehumidifying during the process of waiting for the test, and greatly improve the accuracy of the test.

[0031] See also Figure 4 The method for testing oxygen content of a hygroscopic sample of the present invention uses a hygroscopic sample drying storage box 100 to dry the sample, and comprises the following steps:

[0032] Step S1, opening the bag of sample material and drying it in an oven;

[0033] Step S2, placing the empty sample container 3 on a weighing device to remove the skin, placing a certain mass of dried sample material into the sample container 3 and weighing it on the weighing device, and recording the weight of the sample material, and taking the sample material and the sample container 3 as the first sample;

[0034] Step S3, placing the first sample into the containing groove 22 of the turntable 2, so that the first sample is kept dry in the box body 1;

[0035] Step S4, placing the first sample into a high-frequency infrared oxygen and nitrogen analyzer to measure the oxygen content of the sample material of the first sample;

[0036] Step S5, putting another dried sample material of the same mass into another sample container 3, and recording the weight of the sample material, and taking the sample material and the sample container 3 as the second sample;

[0037] Step S6, during the measurement of the first sample, the second sample is placed in the receiving groove 22 of the turntable 2, and then the turntable 2 is closed to keep the sample material of the second sample dry in the box body 1;

[0038] Step S7, after the test of the first sample is completed, the second sample is taken out from the turntable 2 and placed in the high-frequency infrared oxygen and nitrogen analyzer to measure the oxygen content of the sample material of the second sample.

[0039] The following are specific examples and comparative proportions for illustration:

[0040] Example 1:

[0041] 1. Sample pretreatment: Open the bag of sample coke and dry it in an oven at 80℃ for 1 hour.

[0042] 2. Place the empty nickel crucible on a balance and peel it. Place the dried sample coke in the nickel crucible. The reading on the balance is 0.0156 g. Input the weight of the sample coke into the high-frequency infrared oxygen and nitrogen analyzer.

[0043] 3. Place the nickel crucible containing the sample coke as sample No. 1 into the receiving groove of the turntable, and rotate the turntable to allow sample No. 1 to enter the box body and remain dry.

[0044] 4. After drying, continue to rotate the turntable to rotate sample No. 1 out of the box, put it into the high-frequency infrared oxygen and nitrogen analyzer and set the test parameters of the instrument to conduct oxygen content test.

[0045] 5. During the test of sample No. 1, place another empty nickel crucible on the balance and tar it. Place the dried sample coke in the nickel crucible and read 0.0158 g on the balance.

[0046] 6. Place the nickel crucible containing the sample coke as parallel sample No. 2 into the receiving groove of the turntable, and rotate the turntable to allow sample No. 2 to enter the box body and keep it dry.

[0047] 7. When the test of sample No. 1 is completed, turn the turntable to transfer the parallel sample No. 2, put it into the high-frequency infrared oxygen and nitrogen analyzer, and input the weight of the sample into the high-frequency infrared oxygen and nitrogen analyzer, set the test parameters of the instrument to conduct oxygen content test.

[0048] 8. During the test of sample No. 2, any dried sample can be weighed and placed in a nickel crucible. When the balance reading is stable, record the sample mass and place the nickel crucible with the sample in the receiving slot of the turntable as sample No. 3. Then turn the turntable into the box to keep it dry. Finally, the oxygen content of samples No. 1 and No. 2 was measured to be 2.04% and 2.05% respectively.

[0049] Comparative Example 1:

[0050] 1. Sample pretreatment: Open the bag of sample coke and dry it in an oven at 80℃ for 1 hour.

[0051] 2. Place the empty nickel crucible on a balance and peel it. Weigh 0.0156 g of the dried sample coke and place it in the nickel crucible. When the balance reading stabilizes, enter the sample mass in the high-frequency infrared oxygen and nitrogen analyzer.

[0052] 3. Place the nickel crucible containing the sample coke as sample No. 1 into the instrument for oxygen content testing.

[0053] 4. During the test of sample No. 1, weigh 0.0158 g of the dried sample coke and place it in a nickel crucible. When the balance reading stabilizes, record the sample mass and place the nickel crucible containing the sample as sample No. 2 for testing.

[0054] 5. After the test of sample No. 1 is completed, the weighed sample No. 2 is put into the instrument for testing. The oxygen contents of samples No. 1 and No. 2 are measured to be 2.28% and 2.30% respectively.

[0055] In addition, the equipment test parameters of the high-frequency infrared oxygen and nitrogen analyzer of the present application during the above test are as follows: furnace power: 5500w; carrier gas type: helium; sample introduction: automatic sample introduction; analysis delay: 20s; vacuum opening time: 15s; start baseline: 2s; use comparator level: 1.0%; shortest integration time: 50s; longest integration time: 140s; range selection: automatic; range lower limit: 1950; range upper limit: 2100; cooling time: 5s.

[0056] By comparison, it was found that the moisture content of the two samples dried by the sample drying storage box 100 differed by 0.01%, and the moisture content of the two samples not dried by the sample drying storage box 100 differed by 0.22%. By comparison, it can be seen that the moisture content of the samples dried by the sample drying storage box 100 is lower than that of the samples not dried by the sample drying storage box 100, and the oxygen content test of the samples dried by the sample drying storage box 100 is more accurate.

[0057] The test parameter setting and test principle of the high-frequency infrared oxygen and nitrogen analyzer involved in the moisture-absorbing sample drying storage box 100 of the present invention are well known to ordinary technicians in the field and will not be described in detail here.

[0058] The above disclosure is only a preferred embodiment of the present invention, and certainly cannot be used to limit the scope of rights of the present invention. Therefore, equivalent changes made according to the scope of the patent application of the present invention still fall within the scope covered by the present invention.

Claims

1. A drying storage box for hygroscopic samples, characterized in that: The invention comprises a box body, a turntable, a sample container and a desiccant, wherein an inner cavity is arranged in the box body, an opening communicating with the inner cavity is arranged on one side of the box body, and the turntable is pivotally connected to the box body through a pivot axis so that the turntable can be rotated into or out of the inner cavity through the opening; the pivot axis is parallel to the central axis of the box body and deviates from the central axis of the box body; at least two accommodating grooves are arranged in a concave manner on the upper surface of the turntable, and the sample containers are respectively accommodated in the accommodating grooves; the box body is provided with a partition layer above the inner cavity, and the desiccant is arranged in the partition layer; an air vent communicating with the inner cavity is arranged at the bottom of the partition layer, and an annular sealing ring is arranged at the bottom of the partition layer, and the sealing ring surrounds the outer periphery of the air vent, and when the turntable is located in the inner cavity, the sealing ring is in sealing contact with the outer periphery of the upper surface of the turntable.

2. The hygroscopic sample drying storage box according to claim 1, characterized in that: The upper side of the box body is provided with a cover body which can open or seal the interlayer.

3. The hygroscopic sample drying storage box according to claim 1, characterized in that: Buffer pads are arranged around the opening, and when the rotating disk rotates into or out of the inner cavity, the outer side wall of the rotating disk is in sliding contact with the buffer pads.

4. The hygroscopic sample drying storage box according to claim 1, characterized in that: The pivot axis is located on the outer circumference of the box body.

5. The hygroscopic sample drying storage box according to claim 1, characterized in that: The box body is in a cylindrical structure, and the turntable is in a cylindrical structure.

6. The hygroscopic sample drying storage box according to claim 1, characterized in that: The sample container is a nickel crucible.

7. The hygroscopic sample drying storage box according to claim 1, characterized in that: The upper surface of the turntable is concavely provided with at least two taking-in and putting-out openings symmetrically arranged on both sides of the containing groove, and one side of the taking-in and putting-out openings is communicated with the containing groove.

8. A method for testing oxygen content in hygroscopic samples, characterized in that: The method is carried out using the hygroscopic sample drying storage box according to any one of claims 1 to 7, comprising the following steps: Open the sample bag and dry it in an oven; Putting a certain mass of the dried sample into the sample container and recording it as the first sample; placing the first sample into a high-frequency infrared oxygen and nitrogen instrument to measure the oxygen content of the first sample; Put another dried sample of the same mass into another sample container and record it as the second sample; During the measurement of the first sample, the second sample is placed in the receiving groove of the rotating disk, and then the rotating disk is closed to keep the second sample dry in the box body; After the test of the first sample is completed, the second sample is taken out from the turntable and put into the high-frequency infrared oxygen and nitrogen analyzer to measure the oxygen content of the second sample.

9. The method for testing oxygen content of a hygroscopic sample according to claim 8, wherein: Before placing the sample into the sample container, the empty sample container is placed on a weighing device for taring.

10. The method for testing oxygen content of a hygroscopic sample according to claim 8, wherein: Before placing the first sample into the high-frequency infrared oxygen and nitrogen analyzer, the first sample is placed in the receiving groove of the turntable to keep the first sample dry in the box body.

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