Dry storage box for hygroscopic samples and method for testing oxygen content in samples

Abstract

This invention discloses a moisture-absorbing sample drying and storage box and a method for testing sample oxygen content. The box includes a box body, a turntable, sample containers, and a desiccant. The box body has an inner cavity, and one side of the box body has an opening communicating with the inner cavity. The turntable is pivotally connected to the box body via a pivot shaft. The pivot shaft is parallel to but offset from the central axis of the box body. At least two recessed grooves are formed on the upper surface of the turntable, and the sample containers are respectively placed in these grooves. A partition is provided above the inner cavity in the box body, and the desiccant is disposed within the partition. A vent hole communicating with the inner cavity is formed at the bottom of the partition, and an annular sealing ring is provided at the bottom of the partition, surrounding the outer periphery of the vent hole. This invention provides good sealing performance, effectively preventing sample moisture absorption during testing, improving the accuracy of the measurement, and is convenient to use.

Description

Technical Field

[0001] This invention relates to the field of battery material testing technology, and more particularly to a moisture-absorbing sample drying and storage box and a method for testing sample oxygen content. Background Technology

[0002] In the battery material production process, oxygen content testing is often required. Taking coke as an example, to test the oxygen content of coke, a certain mass of coke sample needs to be taken and placed on a high-frequency infrared oxygen and nitrogen analyzer for measurement. Moreover, for accuracy, multiple samples need to be taken and measured repeatedly, and then the average value is calculated. However, while these samples are waiting to be tested, the untested samples are exposed to moisture and are prone to absorbing moisture, resulting in unstable and high oxygen content data. This leads to inaccurate measurement data and affects the performance of the finished battery. Summary of the Invention

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

[0004] Another objective of this invention is to provide a method for testing the oxygen content of hygroscopic samples with high accuracy, preventing samples from becoming damp while awaiting testing.

[0005] To achieve the above objectives, the present invention provides a moisture-absorbing sample drying and storage box comprising a box body, a turntable, sample containers, and a desiccant. The box body has an inner cavity, and one side of the box body has an opening communicating with the inner cavity. The turntable is pivotally connected to the box body via a pivot shaft, allowing it to rotate into or out of the inner cavity through the opening. The pivot shaft is parallel to and offset from the central axis of the box body. At least two recessed receiving grooves are formed on the upper surface of the turntable, and the sample containers are respectively received in the receiving grooves. A partition is provided above the inner cavity in the box body, and the desiccant is disposed within the partition. A vent hole communicating with the inner cavity is formed at the bottom of the partition, and an annular sealing ring is provided at the bottom of the partition. The sealing ring surrounds the outer periphery of the vent hole, and when the turntable is located within the inner cavity, the sealing ring is in sealing contact with the outer periphery of the upper surface of the turntable.

[0006] Compared with existing technologies, this invention features a rotating turntable within the housing, with at least two recessed receiving slots on its upper surface. These slots accommodate sample containers filled with samples. Since the turntable can rotate into or out of the housing, samples can be fed in or out, enabling rapid sample testing and offering great convenience. Furthermore, the housing's inner cavity has a partition communicating with it, containing a desiccant. A sealing ring at the bottom of the partition seals the turntable, effectively isolating the sample from the outside environment after it is fed into the turntable. Simultaneously, the desiccant dries the sample, effectively preventing moisture buildup during testing and significantly improving test accuracy.

[0007] Preferably, the upper side of the box is provided with a cover that can be opened or sealed to close the compartment. This allows for quick replacement of the desiccant inside the compartment, improving ease of use.

[0008] Preferably, a buffer pad is provided around the opening, and when the turntable rotates into or out of the inner cavity, the outer wall of the turntable slides in contact with the buffer pad. The buffer pad increases the friction between the turntable and the container when the turntable rotates into or out of the container, preventing the sample from flying out due to excessive rotation, and also provides a certain degree of waterproof sealing between the turntable and the container body.

[0009] Preferably, the pivot shaft is located on the outer circumference of the housing. By moving the pivot shaft away from the central axis of the housing, the turntable can be rotated out of the housing at a large angle, thus allowing more samples to be placed on the turntable and increasing the sample capacity of the storage box.

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

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

[0012] Preferably, the upper surface of the turntable has at least two symmetrically arranged pick-and-place ports on both sides of the receiving groove, with one side of each pick-and-place port communicating with the receiving groove. The pick-and-place ports allow fingers or tools to enter, facilitating the removal of the sample container from the receiving groove and improving the ease of handling the sample container.

[0013] A method for testing the oxygen content of hygroscopic samples, using a hygroscopic sample drying and storage box, includes the following steps:

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

[0015] A certain mass of dried sample is placed into the sample container and recorded as the first sample;

[0016] The first sample was placed in a high-frequency infrared oxygen and nitrogen analyzer to determine its oxygen content.

[0017] Another sample of the same mass after drying is placed in another sample container and recorded as the second sample;

[0018] During the measurement of the first sample, the second sample is placed in the receiving slot of the turntable, and then the turntable is turned off to keep the second sample dry in the box.

[0019] After the first sample test is completed, the second sample is removed from the turntable and placed into the high-frequency infrared oxygen and nitrogen meter to determine 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 to remove the tare.

[0021] Preferably, before placing the first sample into the high-frequency infrared oxygen and nitrogen analyzer, the first sample is placed in the receiving slot of the turntable to keep the first sample dry inside the box. Attached Figure Description

[0022] Figure 1 This is a perspective view of the turntable of the sample drying and storage box for determining oxygen content according to the present invention when it is closed.

[0023] Figure 2 This is a diagram showing the state of the turntable of the sample drying and storage box used for determining oxygen content in this invention when it is opened.

[0024] Figure 3 This is an internal cross-sectional view of the sample drying and storage box used in this invention for determining oxygen content.

[0025] Figure 4 This is a flowchart of the method for testing the oxygen content of hygroscopic samples according to the present invention. Detailed Implementation

[0026] To illustrate the technical content, structural features, and effects of the present invention in detail, the following description is provided in conjunction with the embodiments and accompanying drawings.

[0027] like Figures 1 to 3As shown, the moisture-absorbing sample drying and storage box 100 of the present invention includes a box body 1, a turntable 2, a sample container 3, and a desiccant 4. The box body 1 has an inner cavity 11, and one side of the box body 1 has an opening 12 communicating with the inner cavity 11. The turntable 2 is pivotally connected to the box body 1 via a pivot shaft 21, so that the turntable 2 can rotate into or out of the inner cavity 11 through the opening 12. The box body 1 and the turntable 2 are both cylindrical. The pivot shaft 21 is parallel to and offset 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 rotate out of the box body 1 at a large angle, thus allowing more samples to be placed on the turntable 2 and 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 has at least two recessed receiving grooves 22, and the sample containers 3 are respectively housed 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 grooves 22 of the turntable 2 is 9 mm and the depth is 17 mm. The outer diameter of the sample containers 3 is slightly less than 9 mm and the height is 17 mm, so that they can be installed in the receiving grooves 22. The box body 1 is provided with a partition 13 above the inner cavity 11, and the desiccant 4 is disposed in the partition 13; the desiccant 4 is silica gel, molecular sieve or other dehumidifying desiccant. The bottom of the partition 13 has a vent 131 communicating with the inner cavity 11. The bottom of the partition 13 has an annular sealing ring 132 surrounding the vent 131. When the turntable 2 is located inside 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 has a cover 133 that can be opened or sealed to close the partition 13. This allows for quick replacement of the desiccant 4 inside the partition 13, improving ease of use.

[0028] For example Figure 2 and Figure 3 The upper surface of the turntable 2 has at least two symmetrically arranged pick-and-place ports 23 on both sides of the receiving groove 22. One side of each pick-and-place port 23 is connected to the receiving groove 22. The pick-and-place ports 23 allow fingers or tools to enter, thereby facilitating the removal of the sample container 3 from the receiving groove 22 and improving the convenience of picking up and placing the sample container 3.

[0029] Please see Figure 1 and Figure 2A buffer pad 14 is provided around the opening 12. 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 buffer pad 14. The buffer pad 14 is a cotton layer or any material with cushioning and waterproofing effects. The buffer pad 14 increases the friction between the turntable 2 and the box 1 when the turntable 2 rotates into or out of the box 1, preventing the sample from flying out due to excessive rotation of the turntable 2, and also provides a certain degree of waterproof sealing between the turntable and the box 1. The side wall of the turntable 2 exposed through the opening 12 is recessed with a groove or friction protrusion 2a for applying force with fingers to rotate the turntable 2 out of the box 1.

[0030] Compared with the prior art, the present invention, by rotatably arranging a turntable 2 inside the housing 1, and having at least two recessed receiving grooves 22 on the upper surface of the turntable 2, allows the sample container 3 containing the sample to be accommodated using the receiving grooves 22. Since the turntable 2 can rotate into or out of the housing 1, the sample can be fed into or out of the turntable 2, achieving the purpose of rapid sample testing, which is very convenient to use. Furthermore, since a partition 13 communicating with the inner cavity 11 is provided above the inner cavity 11 of the housing 1, and a desiccant 4 is placed inside the partition 13, and a sealing ring 132 sealingly contacts the turntable 2 at the bottom of the partition 13, when the sample is fed into the turntable 2, the sample can be isolated from the outside environment, and the desiccant 4 can dry the sample, thus effectively preventing the sample from becoming damp while waiting for testing, greatly improving the accuracy of the test.

[0031] Please see Figure 4 The method for testing the oxygen content of hygroscopic samples of the present invention utilizes a hygroscopic sample drying and storage box 100 to dry the sample, and includes the following steps:

[0032] Step S1: Open the sample material bag and dry it in an oven;

[0033] Step S2: Place the empty sample container 3 on the weighing device to remove the tare, put a certain mass of dried sample material into the sample container 3 and place it on the weighing device to weigh, and record the weight of the sample material. The sample material and the sample container 3 are used as the first sample.

[0034] Step S3: Place the first sample into the receiving groove 22 of the turntable 2 to keep the first sample dry inside the box 1;

[0035] Step S4: Place the first sample into a high-frequency infrared oxygen and nitrogen analyzer to determine the oxygen content of the sample material of the first sample.

[0036] Step S5: Place another sample material of the same mass after drying into another sample container 3, and record the weight of the sample material. Use 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 1.

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

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

[0040] Example 1:

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

[0042] 2. Place the empty nickel crucible on the balance to remove the tare, put the dried sample coke into the nickel crucible, and read the balance reading as 0.0156g. Input the sample coke weight into the high-frequency infrared oxygen and nitrogen analyzer.

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

[0044] 4. After drying, continue rotating the turntable to rotate sample 1 out of the box, place it in the high-frequency infrared oxygen and nitrogen analyzer, and set the instrument's test parameters to test the oxygen content.

[0045] 5. During the test of sample 1, another empty nickel crucible was placed on the balance to remove the tare, and the dried sample coke was placed in the nickel crucible. The balance reading was 0.0158g.

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

[0047] 7. After sample 1 has finished testing, rotate the turntable to rotate parallel sample 2 out and place it into the high-frequency infrared oxygen and nitrogen analyzer. Input the weight of the sample into the high-frequency infrared oxygen and nitrogen analyzer and set the instrument's test parameters to test the oxygen content.

[0048] 8. During the testing of sample No. 2, any dried sample can be weighed and placed in a nickel crucible. After the balance reading stabilizes, record the sample mass. Place the nickel crucible containing the sample into the receiving slot of the turntable as sample No. 3, and then rotate the turntable into the box to maintain dryness. 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 sample coke bag and dry it in an oven at 80°C for 1 hour.

[0051] 2. Place the empty nickel crucible on the balance to remove the tare, weigh 0.0156g of the dried sample coke into the nickel crucible, and wait for the balance reading to stabilize before inputting the sample mass into the high-frequency infrared oxygen and nitrogen analyzer.

[0052] 3. Place the nickel crucible containing the sample coke into the instrument as sample number 1 for oxygen content testing.

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

[0054] 5. After the test of sample 1 is completed, the weighed sample 2 is placed into the instrument for testing. The oxygen content of samples 1 and 2 is measured to be 2.28% and 2.30%, respectively.

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

[0056] The comparison revealed that the moisture content of the two samples dried in the sample drying and storage box 100 differed by 0.01%, while the moisture content of the two samples not dried in the sample drying and storage box 100 differed by 0.22%. This comparison indicates that the moisture content of the sample dried in the sample drying and storage box 100 was lower than that of the sample not dried in the sample drying and storage box 100, and that the oxygen content test of the sample dried in the sample drying and storage box 100 was more accurate.

[0057] The test parameter settings and test principles of the high-frequency infrared oxygen and nitrogen analyzer involved in the moisture-absorbing sample drying and storage box 100 of this invention are well known to those skilled in the art, and will not be described in detail here.

[0058] The above-disclosed examples are merely preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. Therefore, any equivalent variations made in accordance with the claims of the present invention shall still fall within the scope of the present invention.

Claims

1. A moisture-absorbing sample drying and storage box, characterized in that: The device includes a box body, a turntable, sample containers, and a desiccant. The box body has an inner cavity, and one side of the box body has an opening communicating with the inner cavity. The turntable is pivotally connected to the box body via a pivot shaft, allowing it to rotate into or out of the inner cavity through the opening. The pivot shaft is parallel to and offset from the central axis of the box body. The upper surface of the turntable has at least two recessed receiving grooves, in which the sample containers are respectively received. A partition is located above the inner cavity in the box body, and the desiccant is disposed within the partition. A vent hole communicating with the inner cavity is located at the bottom of the partition, and an annular sealing ring is located at the bottom of the partition, surrounding the outer periphery of the vent hole. When the turntable is located within the inner cavity, the sealing ring is in sealing contact with the outer periphery of the upper surface of the turntable. A buffer pad is provided around the opening, allowing the outer wall of the turntable to slide in contact with the buffer pad when the turntable rotates into or out of the inner cavity.

2. The moisture-absorbing sample drying and storage box as described in claim 1, characterized in that: The upper side of the box is provided with a cover that can be opened or sealed to close the partition.

3. The moisture-absorbing sample drying and storage box as described in claim 1, characterized in that: The pivot shaft is located on the outer circumference of the box.

4. The moisture-absorbing sample drying and storage box as described in claim 1, characterized in that: The box body has a cylindrical structure, and the turntable has a cylindrical structure.

5. The moisture-absorbing sample drying and storage box as described in claim 1, characterized in that: The sample container is a nickel crucible.

6. The moisture-absorbing sample drying and storage box as described in claim 1, characterized in that: The upper surface of the turntable is recessed and has at least two symmetrically arranged pick-up and put-out ports on both sides of the receiving groove, and one side of the pick-up and put-out port is connected to the receiving groove.

7. A method for testing the oxygen content of hygroscopic samples, characterized in that, The process, using the moisture-absorbing sample drying and storage box according to any one of claims 1 to 6, includes the following steps: Open the sample bag and dry it in an oven; A certain mass of dried sample is placed into the sample container and recorded as the first sample; The first sample was placed in a high-frequency infrared oxygen and nitrogen analyzer to determine its oxygen content. Another sample of the same mass after drying is placed in another sample container and recorded as the second sample; During the measurement of the first sample, the second sample is placed in the receiving slot of the turntable, and then the turntable is turned off to keep the second sample dry in the box. After the first sample test is completed, the second sample is removed from the turntable and placed into the high-frequency infrared oxygen and nitrogen meter to determine the oxygen content of the second sample.

8. The method for testing the oxygen content of hygroscopic samples as described in claim 7, characterized in that: Before placing the sample into the sample container, the empty sample container is first placed on a weighing device to remove the tare.

9. The method for testing the oxygen content of hygroscopic samples as described in claim 7, characterized in that: Before placing the first sample into the high-frequency infrared oxygen and nitrogen analyzer, the first sample is placed in the receiving slot of the turntable to keep the first sample dry inside the box.

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