Purity determination system and method

Abstract

The invention discloses a purity determination system and method, and relates to the technical field of chemical analysis detection, a control device is connected with a sample storage device, a solvent storage device and a detergent storage device, corresponding sample output, solvent output and detergent output are controlled and detected, and a solution to be detected is formed through automatic mixing in a reaction device; finally, the conductivity of the solution to be detected is monitored in real time through the detection device, and the purity of the sample is calculated and output according to the amount of the sample, the amount of the solvent and the amount of the detergent. The reaction device is controlled to perform automatic mixing, the detection device is controlled to automatically detect and output the purity of the sample, and the detection precision is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical analysis detection, in particular to a purity determination system and method. BACKGROUND

[0002] Purity determination refers to determining the purity value of high-purity substances (such as high-purity metals, chemical reagents, etc.) through analysis methods. The determination methods are divided into direct method and indirect method, and the former includes liquid chromatography peak area normalization method, direct titration method, etc.

[0003] Common techniques include more than 20 kinds of analysis methods such as high-performance liquid chromatography, gas chromatography, ultraviolet-visible spectrophotometry, etc., among which the differential scanning calorimetry (DSC) method has the characteristics of no need for standard sample, small sample amount (0.04mg detection limit), and is suitable for samples with purity >98%.

[0004] The existing purity measurement methods can be divided into two types: one is direct measurement method, such as using electrolytic method to measure the purity of pure metal, using weight method to measure the purity of pure substance, etc. Since the percentage value of purity is large, the effective number of digits is also large, therefore, the determination method must be high-precision and high-accuracy, which limits the purity determination of high-purity substances. The second is indirect measurement method, which measures the content of various impurities in high-purity substances by high-accuracy and high-sensitivity method, and then subtracts the percentage of the total amount of impurities from the measured substance as the purity of the high-purity substance. The purity determination of high-purity substances mostly adopts this method. There are many methods for measuring impurities in high-purity substances, and the commonly used methods are: ultraviolet-visible spectrophotometry, atomic absorption spectrometry, atomic emission spectrometry, electrochemical analysis method, etc.

[0005] In the existing purity detection, manual operation is mostly relied on, such as manual addition of detergent, observation of reaction end point, which has problems of low efficiency, large error, etc. SUMMARY

[0006] The purpose of the present application is to provide a purity determination system and method, which realizes automatic detection and improves the detection accuracy.

[0007] To solve the above technical problems, the embodiment of the present application provides a purity determination system, which comprises:

[0008] A sample storage device is used for storing the sample to be detected.

[0009] A solvent storage device is used for storing the solvent.

[0010] A detergent storage device is used for storing the detergent.

[0011] A control device connected with the sample storage device, the solvent storage device and the washing agent storage device, for controlling and detecting the sample output of the sample storage device, controlling and detecting the solvent output of the solvent storage device, and controlling and detecting the washing agent output of the washing agent storage device;

[0012] A reaction device for receiving the sample output by the sample storage device, the solvent output by the solvent storage device and the washing agent output by the washing agent storage device, and mixing the sample, the solvent and the washing agent to form a solution to be detected;

[0013] A detection device for monitoring the conductivity of the solution to be detected in real time, and calculating and outputting the purity of the sample according to the amount of the sample, the solvent and the washing agent.

[0014] The sample storage device comprises a liquid sample storage unit, a solid sample storage unit, a sample delivery pump, a sample flow meter, a solid sample grabbing arm and a weighing table. The sample delivery pump is used to output the liquid sample stored in the liquid sample storage unit and detect the flow rate through the liquid sample flow meter. The solid sample grabbing arm is used to grab the stored solid sample from the solid sample storage unit and output it after weighing by the weighing table. The weighing table comprises a first sample weighing table arranged in the solid sample storage unit and a second sample weighing table arranged in the reaction device.

[0015] The reaction device further comprises a heating device arranged therein, for heating the solution to be detected, so that the sample is uniformly distributed in the solvent and the washing agent. The heating device is an ultrasonic heating device, a water bath heating device or an air heating device.

[0016] The reaction device further comprises a funnel arranged therein, for receiving the sample output by the sample storage device, the solvent output by the solvent storage device and the washing agent output by the washing agent storage device, and mixing the sample, the solvent and the washing agent to form a solution to be detected. The funnel is a glass sand core funnel or a filter funnel.

[0017] The reaction device further comprises a waste liquid collection device connected therewith, for collecting the waste liquid after the sample purity detection by the reaction device.

[0018] The application further comprises a housing for integrating the sample storage device, the solvent storage device, the detergent storage device, the control device, the reaction device, and the detection device, and the waste liquid collection device is arranged outside the housing and connected with the waste liquid outlet of the housing, for outputting the waste liquid of the reaction device to the waste liquid collection device through the waste liquid outlet.

[0019] The application further comprises a display device and an operation panel connected with the sample storage device, the solvent storage device, the detergent storage device, the reaction device, the detection device, and the control device, the display device is used for displaying the sample output amount of the sample storage device, the solvent output amount of the solvent storage device, and the detergent output amount of the detergent storage device, and the sample purity value of the detection device, and the operation panel is used for inputting the operation parameters of the sample storage device, the solvent storage device, the detergent storage device, the reaction device, the detection device, and the control device.

[0020] The application further comprises an air compressor connected with the reaction device through a pipeline, and the air compressor is connected with the second heating device, for providing a drying air source for the reaction device.

[0021] The application further comprises a constant temperature device connected with the solvent storage device, for transporting the output solvent to the reaction device after constant temperature treatment in the constant temperature device, and the reaction device is connected with the constant temperature device, for controlling the constant temperature value of the constant temperature device.

[0022] In addition, the embodiment of the application further provides a purity determination method, which adopts the purity determination system as described above, and comprises the following steps:

[0023] S1: mixing a predetermined mass of a sample, a predetermined mass of a solvent, and a predetermined mass of a detergent to form a mixed solution;

[0024] S2: treating the mixed solution at 55-60°C and 30-35 kHz for 10-12 min;

[0025] S3: detecting the conductivity of the mixed solution after stabilization, and calculating the purity value of the sample according to the conductivity, the mass of the sample, the mass of the solvent, and the mass of the detergent;

[0026] S4: performing purity detection on the sample at least three times by using the alcohol washing method, and outputting an alcohol washing purity value;

[0027] S5: calculating whether the error of the purity value relative to the alcohol washing purity value exceeds a threshold value;

[0028] If yes, S6: output an alarm signal, if no, S7: determine that the detection is qualified.

[0029] Compared with the prior art, the purity determination system and method provided by the embodiment of the present application has the following advantages:

[0030] The purity determination system and method provided by the embodiment of the present application are connected with the sample storage device, the solvent storage device and the detergent storage device through the control device, the control and detection of the corresponding sample output, the solvent output and the detergent output are controlled, the to-be-detected solution is automatically mixed in the reaction device, the conductivity of the to-be-detected solution is finally monitored in real time through the detection device, and the purity of the sample is calculated and output according to the amount of the sample, the solvent and the detergent. Since the control device is used to automatically control the automatic output of the corresponding sample, the solvent and the detergent, the reaction device is controlled to automatically mix, and the detection device is controlled to automatically detect and output the purity of the sample, the detection precision is improved. BRIEF DESCRIPTION OF DRAWINGS

[0031] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0032] Figure 1 The structure schematic diagram of one embodiment of the purity determination system provided by the present application;

[0033] Figure 2 The structure schematic diagram of another embodiment of the purity determination system provided by the present application;

[0034] Figure 3 The operation panel structure schematic diagram of one embodiment of the purity determination system provided by the present application;

[0035] Figure 4 The overall process structure schematic diagram of one embodiment of the purity determination method provided by the present application;

[0036] Wherein, 1-outer shell, 2-display device, 3-detergent storage device, 4-ultrasonic heating device, 5-glass sand core funnel, 6-waste liquid collection device, 7-air compressor, 8-solvent storage device, 9-sample storage device, 10-first driving pump, 11-glass sand core funnel fixing frame, 12-funnel cover, 13-second heating device, 14-detection device, 15-constant temperature device, 16-second driving pump. DETAILED DESCRIPTION

[0037] With reference to the drawings of the embodiments of the present application, the technical solutions in the embodiments of the present application will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments of the present application, all the other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0038] Please refer to Figures 1-4 , Figure 1 a structural schematic diagram of an embodiment of a purity determination system provided by the present application; Figure 2 a structural schematic diagram of another embodiment of a purity determination system provided by the present application; Figure 3 a structural schematic diagram of an operation panel of an embodiment of a purity determination system provided by the present application; Figure 4 a structural schematic diagram of a total process of an embodiment of a purity determination method provided by the present application.

[0039] In a specific embodiment, the purity determination system comprises:

[0040] a sample storage device 9 for storing a sample to be detected;

[0041] a solvent storage device 8 for storing a solvent;

[0042] a detergent storage device 3 for storing a detergent;

[0043] a control device connected with the sample storage device 9, the solvent storage device 8 and the detergent storage device 3, for controlling and detecting the sample output amount of the sample storage device 9, controlling and detecting the solvent output amount of the solvent storage device 8, and controlling and detecting the detergent output amount of the detergent storage device 3;

[0044] a reaction device for receiving the sample output by the sample storage device 9, the solvent output by the solvent storage device 8 and the detergent output by the detergent storage device 3, and mixing the sample, the solvent and the detergent to form a solution to be detected;

[0045] a detection device 14 for monitoring the conductivity of the solution to be detected in real time, and calculating and outputting the purity of the sample according to the amount of the sample, the solvent and the detergent.

[0046] The control device is connected with the sample storage device 9, the solvent storage device 8 and the detergent storage device 3, controls and detects the corresponding sample output, solvent output and detergent output, automatically mixes to form a solution to be detected in the reaction device, finally monitors the conductivity of the solution to be detected in real time through the detection device 14, and calculates and outputs the purity of the sample according to the amount of the sample, the solvent and the detergent. Since the control device is used to automatically control the automatic output of the corresponding sample, solvent and detergent, and control the reaction device to automatically mix and control the detection device 14 to automatically detect and output the purity of the sample, the detection precision is improved.

[0047] The structure of the sample storage device 9 is not limited in the application. Since the sample may be a solid or a liquid in actual sample purity detection, in an embodiment, the sample storage device 9 includes a liquid sample storage unit, a solid sample storage unit, a sample delivery pump, a sample flow meter, a solid sample grabbing arm and a weighing table. The sample delivery pump is used to output the liquid sample stored in the liquid sample storage unit and detect the flow through the liquid sample flow meter. The solid sample grabbing arm is used to grab the stored solid sample from the solid sample storage unit and output after weighing by the weighing table. The weighing table includes a first sample weighing table arranged at the solid sample storage unit and a second sample weighing table arranged at the reaction device.

[0048] The liquid sample storage unit and the solid sample storage unit are arranged to store liquid samples and solid samples respectively, so that the detection capability for different types of samples is improved, and the adaptability of the system is improved.

[0049] The sample delivery pump and the sample flow meter are used to deliver and measure the liquid sample, so that the accuracy of the delivery of the liquid sample is ensured, and the purity detection precision is improved. The solid sample grabbing arm is used to transfer and output the solid sample, and the weighing table is used to detect the weight of the solid sample storage unit and the reaction device, so that the detection precision of the solid sample is improved. For example, the input amount of the solid sample in the reaction device can be obtained according to the weight increase of the reaction device, the weight reduction amount of the solid sample in the solid sample storage unit can be obtained according to the weight reduction of the solid sample storage unit detected by the first sample weighing table arranged at the solid sample storage unit, and whether there is a device failure can be verified according to the comparison between the first sample weighing table and the second sample weighing table, so that the quality of the sample is accurately detected.

[0050] Similarly, the weight change can also be used to detect the liquid sample, so that the detection precision is improved.

[0051] This application includes, but is not limited to, the above-described sample delivery and testing methods; other structures may also be employed.

[0052] To further improve detection speed and accuracy, in one embodiment, the purity determination system further includes a heating device disposed in the reaction apparatus for heating the solution to be tested, so that the sample is uniformly distributed in the solvent and the detergent. The heating device is an ultrasonic heating device 4, a water bath heating device, or an air heating device.

[0053] By setting a heating device in the reaction apparatus to heat the solution to be tested, the sample is uniformly distributed in the solvent and the detergent, which allows the solution to be tested to be mixed quickly and evenly, thereby improving the detection accuracy of the subsequent detection device 14.

[0054] This application does not limit the type of heating device, which may be an ultrasonic heating device, a water bath heating device, an air heating device, or other heating devices.

[0055] The ultrasonic heating device 4 uses ultrasound for heating, which can achieve non-contact heating. Water bath heating only requires contact with the outside of the reaction device. Air heating only requires passing heated air into the solution to be tested in the reaction device, which can achieve both heating and stirring of the solution to be tested, thus improving detection efficiency.

[0056] To further achieve efficient mixing of different samples with other solvents, in one embodiment, the purity determination system further includes a funnel disposed in the reaction device for receiving the sample output from the sample storage device 9, the solvent output from the solvent storage device 8, and the detergent output from the detergent storage device 3, and mixing the sample, the solvent, and the detergent to form a solution to be tested. The funnel is a glass frit funnel or a filter funnel.

[0057] By setting a funnel in the reaction apparatus to receive the sample, solvent, and detergent for mixing to form the solution to be tested, the mixing efficiency is improved.

[0058] This application does not limit the type, shape, or size of the funnel.

[0059] To further reduce residual contamination, minimize the impact on subsequent tests, and improve testing accuracy, in one embodiment, the purity determination system further includes a waste liquid collection device 6 connected to the reaction apparatus for collecting waste liquid after the reaction apparatus performs sample purity testing.

[0060] By connecting the waste liquid collection device 6 to the reaction apparatus, the waste liquid generated after sample purity testing is collected, improving environmental friendliness. Simultaneously, the discharge of this waste liquid avoids affecting subsequent sample testing, thus improving testing accuracy.

[0061] In addition, this application may also include multiple reactors in the reaction device, different detectors in different sample tests, and after a sample test is completed, the reactor can be directly removed from the reaction device and replaced with a new reactor, thereby reducing the impact on the reaction device. The cleaning of the reactor and the discharge and treatment of non-waste liquids are also performed outside the reaction device, or other methods are used, etc., which are not limited in this application.

[0062] This application does not limit the structure, material, size, or collection method of the waste liquid collection device 6. It can be used for simple waste liquid collection, or it can be used to perform harmless treatment on the waste liquid collection device 6 according to the type of waste liquid before discharge.

[0063] To further improve the ease of use of the system, in one embodiment, the purity determination system further includes an outer housing 1 for integrating the sample storage device 9, the solvent storage device 8, the detergent storage device 3, the control device, the reaction device, and the detection device 14. The waste liquid collection device 6 is disposed outside the outer housing 1 and connected to the waste liquid outlet of the outer housing 1, for discharging the waste liquid of the reaction device to the waste liquid collection device 6 through the waste liquid outlet.

[0064] By integrating the sample storage device 9, the solvent storage device 8, the detergent storage device 3, the control device, the reaction device, and the detection device 14 into the outer casing 1 to form a whole, it can be moved freely and sample purity detection can be performed at any position without having to disconnect the connections of each component and then reassemble them at a new position, thus improving efficiency and convenience.

[0065] This application does not limit the structure of the outer shell 1, and can provide snap-fit ​​parts, bolt holes, etc. inside it to fix the various components, thereby improving the efficiency of use.

[0066] To further monitor and control the purity testing process, in one embodiment, the purity determination system further includes a display device 2 and an operation panel connected to the sample storage device 9, the solvent storage device 8, the detergent storage device 3, the reaction device, the detection device 14, and the control device. The display device 2 displays the sample output of the sample storage device 9, the solvent output of the solvent storage device 8, the detergent output of the detergent storage device 3, and the sample purity value of the detection device 14. The operation panel is used to input the operating parameters of the sample storage device 9, the solvent storage device 8, the detergent storage device 3, the reaction device, the detection device 14, and the control device.

[0067] By setting up display device 2 to display the operating parameters of each component, the current operating status of each device can be obtained, improving management efficiency. By setting up the operation panel, the operating parameters of each component in the purity testing process can be set, allowing for corresponding values ​​based on different testing parameters, thus improving testing accuracy and efficiency.

[0068] In this application, there is no limitation on the method of setting the parameters of the corresponding device through the operation panel. It can be to directly set specific parameters, or to use a similar mode to directly select the sample type to be tested and automatically generate the corresponding parameter scheme, etc.

[0069] Since solvent or even residue from previous samples may remain in the corresponding pipelines after sample testing, they need to be cleaned. After cleaning, water droplets may remain, affecting the next sample test. Furthermore, bacterial contamination may occur if the system is not used for a long time. In one embodiment, the purity determination system also includes an air compressor 7 connected to the reaction device via a pipeline. The air compressor 7 is connected to the second heating device 13 to provide a drying air source for the reaction device.

[0070] By setting up an air compressor 7 and connecting it to the second heating device 13, a drying air source is provided for the reaction device. After cleaning is completed, the pipeline can be quickly dried using the drying air source, which improves cleaning efficiency, facilitates rapid preparation for the next sample test, reduces the testing cycle, and improves testing efficiency.

[0071] This application does not limit the structure of the air compressor 7 and the second heating device 13. This application includes, but is not limited to, the drying air source supply equipment mentioned above.

[0072] In order to accurately control the dissolution process of the sample, in one embodiment, the purity determination system further includes a constant temperature device 15 connected to the solvent storage device 8, which is used to deliver the output solvent to the reaction device after being constant temperature treated by the constant temperature device 15. The reaction device is connected to the constant temperature device 15 and is used to control the constant temperature value of the constant temperature device 15.

[0073] By connecting the solvent storage device 8 to the temperature control device 15, the output solvent is subjected to temperature control treatment in the temperature control device 15 and then transported to the reaction device, so that the temperature is consistent before forming a solution with the sample, thereby reducing the detection accuracy error caused by errors.

[0074] This application does not limit the temperature control device 15, the specific temperature control method, or the duration of the solvent's presence in the temperature control device.

[0075] In one embodiment, the purity determination system includes: an outer casing 1 with a display screen and operation panel on top, and an internal detergent storage device 3 for storing detergent and installing air for the air purging pipeline; an ultrasonic heating device 4 with a built-in temperature control and ultrasonic generator for heating and dispersing the sample; a glass frit funnel 5, located in the reaction device, working in conjunction with the glass frit holder 11 and the funnel cover 12 for ultrasonic cleaning of the sample within the glass frit funnel 5; an external waste liquid recovery device connected to the reaction tank via a pipeline for collecting waste liquid; an air compressor 7 providing drying air via a second heating device 13; an internal solvent storage device 8 providing appropriate solvent, deionized water, and air for the air purging pipeline to the glass frit funnel 5; and a sample storage device 9 providing liquid sample to the entire pipeline. The system includes an automatic sample injection device, a deionized water and air purging pipeline; a second heating device 13, used to heat the gas in the air compressor 7 to provide a drying gas source for the glass frit funnel; a detection device 14, which monitors the electrical signal in the solution in real time, detects the content of filtered impurities and performs purity conversion; a constant temperature device 15, into which solvent is injected in proportion according to the detection requirements, subjected to constant temperature treatment, and then transferred to the first drive pump 10 via the second drive pump 16, and then transferred to the glass frit funnel for reaction; and a control device, electrically connected to the display screen, sample storage device 9, solvent storage device 8, detergent storage device 3, ultrasonic heating device 4, detection device 14, heating device, constant temperature device 15, waste liquid recovery device 6, air compressor 7, first drive pump 10, and second drive pump 16, to achieve automated operation.

[0076] The sample storage device 9 includes four liquid inlet pipes and one air inlet pipe, which are connected to the glass frit funnel via the first drive pump 10; the solvent storage device 8 includes four liquid inlet pipes and one air inlet pipe, which are connected to the glass frit funnel via the first drive pump 10 or the second drive pump 16 and the constant temperature device 15; the detergent storage device 3 includes four liquid inlet pipes and one air inlet pipe, which are connected to the glass frit funnel via the first drive pump 10 or the second drive pump 16 and the constant temperature device 15.

[0077] The temperature control of the ultrasonic heating device 4 has an adjustable temperature range of 25℃–100℃ and an ultrasonic frequency of 20kHz–40kHz. The air compressor 7 provides pneumatic power and assists in solvent delivery. The second heating device 13 is used to heat the gas in the air compressor 7 to provide a drying gas source for the glass frit funnel.

[0078] The detection device 14 monitors the electrical signal in the solution in real time, detecting the content of filtered impurities and performing purity conversion. The waste liquid recovery device is connected to the reaction tank via a pipeline for collecting waste liquid.

[0079] The control device controls the liquid sample injection volume, solvent injection volume, detergent injection volume, ultrasonic heating time, detection time, electrical signal recognition and conversion, and waste liquid recovery sequence through a preset program.

[0080] For solid powder samples, after being added to the glass frit funnel manually or mechanically, the control device controls the solvent injection volume, detergent injection volume, ultrasonic heating time, detection time, electrical signal recognition and conversion, and waste liquid recovery sequence through a preset program.

[0081] In one embodiment, the powder sample to be tested is placed in a glass frit funnel, and the control device starts the drive pump to inject detergent according to the program; the ultrasonic heating device 4 treats the sample at 60°C and 30kHz for 10 minutes; the detection device 14 monitors the electrical signal in the solution in real time to detect the content of filtered impurities and perform purity conversion. Waste liquid is collected by a waste liquid recovery device, and purity data is output through a display screen.

[0082] In another embodiment, the liquid sample to be tested is placed in the sample storage device 9 and injected into the glass frit funnel by the first drive pump 10; the solvent is injected according to the procedure and transferred to the constant temperature device 15 for preheating by the second drive pump 16, and then injected into the glass frit funnel by the first drive pump 10; the ultrasonic heating device 4 processes the solution at 60°C and 30kHz for 10 minutes; the electrical signal in the solution is monitored in real time by the detection device 14 to detect the chloride ion impurity content and purity conversion; the waste liquid is collected by the waste liquid recovery device, and the purity data is output through the display screen.

[0083] To verify the accuracy of the purity test, the alcohol washing method was used as a comparative experiment. The procedure is as follows:

[0084] 1. Weigh 2g of the untreated sample (accurate to 0.0001g) into a 300mL beaker, add 50mL of 80% ethanol preheated to 60℃~65℃, stir to dissolve, and filter the upper solution through a glass frit filter of known mass. Repeat the same operation three times, transferring all insoluble matter into the glass frit filter. Further wash the insoluble matter in the filter with 80% ethanol at 60℃~65℃ until the filtrate is free of chloride ions (tested with silver nitrate solution; the total amount of ethanol used for washing is approximately 250mL), and filter slowly under vacuum. Wash the insoluble matter in the glass filter three times with 50mL of 95% ethanol, and finally remove the water from the insoluble matter with 50mL of anhydrous ethanol in several portions. Dry at 105℃±2℃ for 2h (loosening once with a stainless steel spatula during this time). Cool to room temperature in a desiccator and weigh (accurate to 0.0001g).

[0085] 2. Purity calculation formula: Purity = mass of insoluble matter / mass of sample.

[0086] Table 1 below shows the structural comparison of multiple experiments and corresponding comparative experiments.

[0087] Serial number Purity of group 3 (%) Purity of group 4 (%) Purity of group 5 (%) Purity of group 6 (%) Purity of group 7 (%) Systematic error (%) Detection time (min) Example 92.46 92.43 92.47 92.53 92.45 ±0.1 15 Comparative example 92.25 92.70 92.60 92.53 92.15 ±0.6 150

[0088] Table 1

[0089] Analysis of the experimental data shows that the error rate of the traditional manual detection method is ±0.6%, while the error rate of the present invention is reduced to ±0.1%, and the detection time is reduced from 150 minutes to 15 minutes.

[0090] Therefore, the above-mentioned device has beneficial effects;

[0091] High degree of automation, reducing human intervention;

[0092] Ultrasonic dispersion improves reaction uniformity;

[0093] Waste liquid recycling avoids environmental pollution.

[0094] In addition, embodiments of this application also provide a purity determination method, employing the purity determination system described above, including:

[0095] S1: A mixed solution is formed by mixing a predetermined mass of sample, a predetermined mass of solvent, and a predetermined mass of detergent.

[0096] S2: Treat the mixed solution at 55℃-60℃ and 30kHz-35kHz for 10min-12min;

[0097] S3: Detect the conductivity of the mixed solution after stabilization, and calculate the purity value of the sample based on the conductivity, the mass of the sample, the mass of the solvent, and the mass of the detergent;

[0098] S4: After performing at least three purity tests on the sample using the alcohol washing method, output the alcohol washing purity value;

[0099] S5: Calculate whether the error of the purity value relative to the alcohol-washed purity value exceeds a threshold;

[0100] If yes, S6: Output an alarm signal; if no, S7: Determine that the test is qualified.

[0101] Since the purity determination method uses the purity determination system described above and has the same beneficial effects, this application will not elaborate on it further.

[0102] In summary, the purity determination system and method provided in this embodiment of the invention connects a control device to a sample storage device, a solvent storage device, and a detergent storage device. This control device controls and detects the corresponding output amounts of sample, solvent, and detergent. The components are automatically mixed in a reaction device to form a solution to be tested. Finally, a detection device monitors the conductivity of the solution in real time and calculates and outputs the purity of the sample based on the amounts of sample, solvent, and detergent. Because the control device automatically controls the output of the corresponding sample, solvent, and detergent, and controls the automatic mixing in the reaction device and the detection device to automatically detect and output the purity of the sample, the detection accuracy is improved.

[0103] The purity determination system and method provided by this invention have been described in detail above. Specific examples have been used to illustrate the principles and implementation methods of this invention. The descriptions of the embodiments above are only for the purpose of helping to understand the method and core ideas of this invention. It should be noted that those skilled in the art can make various improvements and modifications to this invention without departing from its principles, and these improvements and modifications also fall within the protection scope of the claims of this invention.

Claims

1. A purity determination system, characterized in that, include; Sample storage device for storing samples to be tested; Solvent storage device for storing solvents; Detergent storage device for storing detergent; A control device, connected to the sample storage device, the solvent storage device, and the detergent storage device, is used to control and detect the sample output of the sample storage device, control and detect the solvent output of the solvent storage device, and control and detect the detergent output of the detergent storage device. A reaction apparatus is used to receive the sample output from the sample storage device, the solvent output from the solvent storage device, and the detergent output from the detergent storage device, and to mix the sample, the solvent, and the detergent to form a solution to be tested; The detection device is used to monitor the conductivity of the solution to be tested in real time, and to calculate and output the purity of the sample based on the amount of the sample, the solvent and the detergent.

2. The purity determination system as described in claim 1, characterized in that, The sample storage device includes a liquid sample storage unit, a solid sample storage unit, a sample delivery pump, a sample flow meter, a solid sample gripping arm, and a weighing platform. The sample delivery pump is used to output the liquid sample stored in the liquid sample storage unit and detect the flow rate through the liquid sample flow meter. The solid sample gripping arm is used to grab the fixed sample stored in the solid sample storage unit, weigh it through the weighing platform, and output it. The weighing platform includes a first sample weighing platform installed in the solid sample storage unit and a second sample weighing platform installed in the reaction device.

3. The purity determination system as described in claim 1, characterized in that, It also includes a heating device disposed in the reaction apparatus for heating the solution to be tested, so that the sample is uniformly distributed in the solvent and the detergent. The heating device is an ultrasonic heating device, a water bath heating device or an air heating device.

4. The purity determination system as described in claim 1, characterized in that, It also includes a funnel disposed in the reaction apparatus for receiving the sample output from the sample storage device, the solvent output from the solvent storage device, and the detergent output from the detergent storage device, and mixing the sample, the solvent, and the detergent to form a solution to be tested. The funnel is a glass frit funnel or a filter funnel.

5. The purity determination system as described in claim 4, characterized in that, It also includes a waste liquid collection device connected to the reaction apparatus for collecting waste liquid after the reaction apparatus has performed sample purity testing.

6. The purity determination system as described in claim 5, characterized in that, It also includes a housing for integrating the sample storage device, the solvent storage device, the detergent storage device, the control device, the reaction device, and the detection device. The waste liquid collection device is disposed outside the housing and connected to the waste liquid outlet of the housing, for discharging the waste liquid of the reaction device to the waste liquid collection device through the waste liquid outlet.

7. The purity determination system as described in claim 6, characterized in that, It also includes a display device and an operation panel connected to the sample storage device, the solvent storage device, the detergent storage device, the reaction device, the detection device, and the control device. The display device is used to display the sample output volume of the sample storage device, the solvent output volume of the solvent storage device, the detergent output volume of the detergent storage device, and the sample purity value of the detection device. The operation panel is used to input the operating parameters of the sample storage device, the solvent storage device, the detergent storage device, the reaction device, the detection device, and the control device.

8. The purity determination system as described in claim 1, characterized in that, It also includes an air compressor connected to the reaction apparatus via a pipeline, the air compressor being connected to a second heating device for providing a drying air source for the reaction apparatus.

9. The purity determination system as described in claim 1, characterized in that, It also includes a temperature control device connected to the solvent storage device, used to deliver the output solvent to the reaction device after being subjected to temperature control treatment in the temperature control device. The reaction device is connected to the temperature control device and is used to control the temperature value of the temperature control device.

10. A method for determining purity, characterized in that, The purity determination system according to any one of claims 1-9 comprises: S1: A mixed solution is formed by mixing a predetermined mass of sample, a predetermined mass of solvent, and a predetermined mass of detergent. S2: Treat the mixed solution at 55℃-60℃ and 30kHz-35kHz for 10min-12min; S3: Detect the conductivity of the mixed solution after stabilization, and calculate the purity value of the sample based on the conductivity, the mass of the sample, the mass of the solvent, and the mass of the detergent; S4: After performing at least three purity tests on the sample using the alcohol washing method, output the alcohol washing purity value; S5: Calculate whether the error of the purity value relative to the alcohol-washed purity value exceeds a threshold; If yes, S6: Output an alarm signal; if no, S7: Determine that the test is qualified.

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