Gypsum clinker phase composition testing system and method

Abstract

The invention discloses a testing system and method for gypsum clinker phase composition. The testing system for the gypsum clinker phase composition comprises a sampling device, one or more testing devices and an analysis-transmission-storage device, wherein one end of the sampling device is connected with gypsum production line equipment, and the other end of the sampling device is connected with the one or more testing devices through one or more sample conveying pipelines; the analysis-transmission-storage device is used for analyzing and summarizing test results during the test period and after the test is completed, and determining the phase composition of the gypsum clinker. The system and the method can overcome the defects that time and labor are wasted and errors of test results are large during analysis of gypsum clinker phase determination in the prior art, can also overcome the problem that rapid and accurate determination cannot be achieved at the same time, achieve the purpose of rapid and accurate determination of gypsum clinker phase composition on a production line, and have guiding significance for actual production of gypsum clinker.

Description

Technical Field

[0001] The present invention relates to but is not limited to the technical field of a new type of building material, and in particular to but is not limited to a testing system and method for rapidly and accurately determining the phase composition of gypsum clinker. Background Art

[0002] There are five forms and seven variants of gypsum phase. The preparation process of gypsum cementitious materials is mainly the process of heating dihydrate gypsum to dehydrate it and transform it into different dehydrated gypsum phases. In the process of dihydrate gypsum transforming into dehydrated phase, because hemihydrate gypsum and type III anhydrous gypsum are metastable compounds, there is no very definite phase transition point. The preparation process of gypsum powder from different origins is not the same. The quality of gypsum powder prepared by different production processes varies greatly. Real-time monitoring of the proportion of each phase of gypsum on the production line is very important for adjusting process parameters and preparing gypsum products that can meet different production needs.

[0003] At present, there are two main methods for phase analysis of gypsum cementitious materials: oven method (A method) and moisture meter method (B method). Both methods are derived from the principle of gypsum dehydration at different temperatures, but each has its own advantages and disadvantages. The oven method is more accurate, but it takes a long time and cannot meet the needs of rapid real-time monitoring of production; although the moisture meter is fast, its test results have large errors and cannot quickly provide accurate test data for the production line.

[0004] Therefore, in the industrial production process, it is of great significance to develop a fast and accurate testing system and analysis method that can realize online monitoring of the phase composition of gypsum cementitious materials prepared under different calcination process conditions. Summary of the invention

[0005] Based on this, this patent aims to overcome the shortcomings of the oven method and the moisture meter method, and develop a fast and accurate testing system and method that can provide monitoring data for the production line.

[0006] The purpose of the present application is to provide a testing system and method for rapidly and accurately determining the phase composition of gypsum clinker. The system and method can overcome the shortcomings of the prior art that the phase analysis of gypsum clinker is time-consuming and labor-intensive, and the test results have large errors, and can also overcome the problem that it cannot achieve both rapidity and accuracy at the same time, and achieve the purpose of rapidly and accurately determining the phase composition of gypsum clinker on the production line, which has guiding significance for the actual production of gypsum clinker.

[0007] In order to achieve the above-mentioned objectives, the first aspect of the present application provides a testing system for the phase composition of gypsum clinker, wherein the testing system for the phase composition of gypsum clinker comprises: a sampling device, one or more testing devices and an analysis-transmission-storage device.

[0008] In an exemplary embodiment, one end of the sampling device is connected to the gypsum production line to achieve real-time sampling; the other end is connected to the one or more testing devices to ensure that the sample can be transported to the one or more testing devices according to the test requirements.

[0009] In an exemplary embodiment, the other end of the sampling device is connected to the one or more testing devices through one or more sample transport pipes.

[0010] In an exemplary embodiment, the analysis-transmission-storage device is configured to analyze and summarize the test results during and after the test to determine the phase composition of the gypsum clinker.

[0011] In an exemplary embodiment, the analysis-transmission-storage device includes a computer, and the sampling device and the testing device are respectively connected to the analysis-transmission-storage device, and are used to control the sampling device and the testing device to perform sampling and measurement respectively, to achieve simultaneous online analysis and testing of multiple samples, and to summarize, store and feedback the test results.

[0012] In an exemplary embodiment, the sampling device is vacuum-connected to the gypsum production line via a vacuum pump.

[0013] In an exemplary embodiment, the sampling device comprises:

[0014] A connection port, used to connect the sampling device to a gypsum production line;

[0015] A sampling and preserving device, which is connected to the connection port and is used to obtain, retain and preserve the sample;

[0016] A connecting pipe connects the connection port and the sampling storage container.

[0017] In an exemplary embodiment, a sealing device is provided at the front end of the connecting pipe for sealingly connecting the connecting port to the connection of the gypsum production line or the location where sampling is required; the vacuum pump is connected to the side of the connecting pipe.

[0018] In an exemplary embodiment, the sample holder further includes a program control system.

[0019] In an exemplary embodiment, the sampling container further includes a vacuum control device and a temperature and humidity control device for controlling the vacuum degree and the temperature and humidity in the sampling container so as to store the sample under vacuum, cooling and humidity control.

[0020] In an exemplary embodiment, the sampling holder includes: a hanging table, a sampling channel, a sampler, a sample storage table and a sample storage; wherein the hanging table is arranged on the front baffle in the sampling holder and is located at the upper part of the interface between the connecting pipe and the sampling holder; the sampler is hung on the hanging table; the sampling channel connects the sampler and the interface; the sample storage table is arranged on the rear baffle in the sampling holder, and the sample storage is located on the sample storage table, and is used to complete the storage and numbering of the samples to be tested.

[0021] In an exemplary embodiment, the sampler is a sampling cavity that can be opened and closed on both sides, and includes: a telescopic arm connected to the hanging platform, a sampling spoon located in the sampler, and a spring connected to the sampling spoon.

[0022] In an exemplary embodiment, a translation device is provided at the bottom of the sample storage table, and the sample storage table is translated between the sampler and the rear baffle through the translation device.

[0023] In an exemplary embodiment, the sample storage station may be provided with one or more sample storage containers.

[0024] In an exemplary embodiment, a plurality of parallel sample storage stations may be provided in the sampling holder.

[0025] In an exemplary embodiment, the program control system can control: the telescopic arm to deliver the sampler to the interface, the opening and closing of the sampling cavity, the movement of the sample storage table, and the linkage between the sampling holder and the testing device.

[0026] In an exemplary embodiment, the sampling holder is connected to the testing device via the one or more sample transport pipes.

[0027] In an exemplary embodiment, the test device is a drying test device, which includes a drying box and one or more weighing devices, wherein the weighing devices are located on the top of the outer side of the drying box and are thermally insulated from the drying box.

[0028] In an exemplary embodiment, the weighing device is provided with a suspension rod and a sample placing device, a through hole for accommodating the suspension rod to pass through is provided on the top of the drying box, and the sample placing device is suspended on the suspension rod and suspended in the drying box for weighing the sample.

[0029] In an exemplary embodiment, the sample placing device is a weighing pan or a weighing bottle located on the weighing pan.

[0030] In an exemplary embodiment, the drying temperature of the drying oven can be set according to test requirements. For example, the drying temperature of the drying oven can be set to 40-45°C or 220-240°C.

[0031] In an exemplary embodiment, the vacuum degree of the drying oven can be set as needed. Optionally, the vacuum degree of the drying oven can be -0.07 MPa to -0.09 MPa.

[0032] In an exemplary embodiment, the number of the testing devices may be 3, and each of the testing devices may be used to measure the content of soluble type III anhydrous gypsum, hemihydrate gypsum and dihydrate gypsum respectively.

[0033] In an exemplary embodiment, in each of the testing devices, the number of the weighing devices may be 6.

[0034] In an exemplary embodiment, the drying box may also include a sample cleaning and processing device for cleaning and preserving samples after the test is completed.

[0035] A second aspect of the present application provides a method for testing the phase composition of gypsum clinker, which adopts the above-mentioned testing device for the phase composition of gypsum clinker.

[0036] In an exemplary embodiment, the method comprises the following steps:

[0037] 1) Connect the sampling device to the gypsum production line;

[0038] 2) Sampling and preservation: the sampling device samples and preserves the gypsum clinker samples in the gypsum production line;

[0039] 3) Testing: regularly transporting the gypsum clinker samples from the sampling device to one or more testing devices through one or more sample transport pipelines, and performing simultaneous drying and weighing tests on the multiple gypsum clinker samples in the testing devices;

[0040] 4) Displaying the results: The calculation formula is input into the analysis-transmission-storage device in advance. After the test is completed, the test results are analyzed and summarized by the analysis-transmission-storage device to determine the phase composition of the gypsum clinker.

[0041] In an exemplary embodiment, step 1) includes: before connecting the connecting pipe of the sampling preserver and the discharge port (or sampling port) of the gypsum production line, first seal the connecting pipe, start the vacuum pump to evacuate the connecting pipe, the sampling device, and the testing device; when the vacuum degree reaches the working condition, stop vacuuming, connect and communicate the sealed connecting pipe and the discharge port or sampling port of the gypsum production line, so as to realize the overall connection between the sampling device and the gypsum production line.

[0042] In an exemplary embodiment, the vacuum degree of the vacuum pump may be -0.07 MPa to -0.09 MPa.

[0043] In an exemplary embodiment, step 2) includes: when sampling, the program control system controls the telescopic arm to send the sampler to the interface between the connecting pipe and the sampling holder through the sampling channel, at this time, the side of the sampler adjacent to the interface is opened, and the spring in the sampling holder ejects the sampling spoon in the sampler to the discharge port (or sampling port) for sampling; after sampling, the spring contracts to retract the sampling spoon into the sampler, at this time, the side of the sampler adjacent to the interface is closed, and the telescopic arm retracts the sampler to the hanging table to complete the sampling;

[0044] When storing samples, the program control system controls the translation device at the bottom of the sample storage table to translate the sample storage table to the sampler, and the sampler opens on a side adjacent to the sample storage table. The spring pops out the sampling spoon and places the sample in the sample storage of the sample storage table. Subsequently, the spring contracts to retract the sampling spoon into the sampler. At this time, the sampler closes on a side adjacent to the sample storage table, and the translation device translates the sample storage table to the rear baffle of the sampling holder to complete the storage of the sample, and seals and cools it down.

[0045] In an exemplary embodiment, step 3) includes:

[0046] When the test program is started, the test device completes all the preparatory work before the test;

[0047] The sample in the sample storage device is transported to the sample placing device of the weighing device through the sample transport pipeline;

[0048] The drying box is evacuated and a heating program is started, and the evacuation is stopped when the vacuum degree of the drying box reaches the working condition and the temperature reaches the set value; heating is continued for a period of time, nitrogen is introduced into the drying box until the air pressure in the drying box is the same as the external atmospheric pressure, and the total weight of the placement device is weighed; optionally, the heating time is continued for 0.5h or 1h;

[0049] This process is repeated, and the sample placing device is weighed periodically until it reaches a constant weight, and the test is completed. Optionally, the constant weight is reached when the difference between two weighings with a heating time interval of 0.5 h or 1 h is no more than 0.5 g.

[0050] In an exemplary embodiment, the preparatory work before the test includes: evacuating the drying box and repeatedly weighing until the sample placement device reaches a constant weight.

[0051] In an exemplary embodiment, in step 3), the drying temperature of the drying oven can be set according to test requirements, for example, the drying temperature of the drying oven can be set to 40-45°C or 220-240°C.

[0052] In an exemplary embodiment, in step 3), the vacuum degree of the drying oven can be set as needed. Optionally, the vacuum degree of the drying oven can be -0.07 MPa to -0.09 MPa.

[0053] In an exemplary embodiment, in step 3), the drying ovens in the testing device are drying oven A, drying oven B and drying oven C, which are used to determine the content of soluble type III anhydrous gypsum, hemihydrate gypsum and dihydrate gypsum, respectively.

[0054] In an exemplary embodiment, in step 3), the drying temperature of the drying oven A is 230±3°C, the drying temperature of the drying oven B is 40±3°C, and the drying temperature of the drying oven C is 40±4°C.

[0055] In an exemplary embodiment, when the drying oven is a drying oven A, step 3) further includes:

[0056] The drying box A is connected to a first normal temperature dryer and a sealing and heat-insulating device is provided between the drying box A and the first normal temperature dryer;

[0057] The weighing bottle in the drying oven A is covered with a bottle cap, the sealing and heat-insulating device is closed, and the drying oven A is evacuated and a heating program is started;

[0058] When the vacuum degree of the drying box A reaches the working condition and the temperature reaches the set value, stop the vacuuming, open the bottle cap and place it on the weighing pan for heating; continue heating for a period of time, introduce nitrogen into the drying box A until the air pressure in the drying box A is the same as the external atmospheric pressure, and weigh the total weight of the placement device;

[0059] Repeat this process and regularly weigh the weighing bottle in the drying oven A until it reaches a constant weight.

[0060] After the heating is completed, the sealed heat-insulating device is opened, and the weighing bottle in the drying box A is transported to the first normal-temperature dryer for cooling.

[0061] In an exemplary embodiment, when the drying oven is a drying oven B, step 3) further includes:

[0062] The drying box B is connected to a first liquid storage cylinder containing 95% ethanol solution; the drying box B is connected to a second normal temperature dryer, and sealing and heat insulation devices are respectively provided between the drying box B and the first liquid storage cylinder and the second normal temperature dryer;

[0063] Slowly add 95% ethanol solution along the edge of the weighing bottle in the drying oven B, shake gently to make the sample in the drying oven B evenly moistened and let it stand;

[0064] The weighing bottle in the drying oven B is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven B is evacuated and the heating program is started; when the vacuum degree of the drying oven B reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on a weighing pan for heating; the heating is continued for a period of time, nitrogen is introduced into the drying oven B until the air pressure in the drying oven B is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed;

[0065] Repeat this process and regularly weigh the weighing bottle in the drying oven B until it reaches a constant weight.

[0066] When the weighing bottle in the drying box B is heated for ≥6 hours, the sealing and heat-insulating device is opened, the weighing bottle is covered and moved into the second normal-temperature dryer for cooling to room temperature.

[0067] In an exemplary embodiment, when the drying oven is a drying oven C, step 3) further includes:

[0068] The drying box C is connected to a second liquid storage cylinder containing distilled water, and the drying box C is also connected to a third normal temperature dryer. Sealing and heat insulation devices are respectively provided between the drying box C and the second liquid storage cylinder and the third normal temperature dryer;

[0069] Slowly add distilled water along the edge of the weighing bottle of the drying oven C, and shake gently to make the sample in the drying oven C evenly moistened and soaked;

[0070] The weighing bottle in the drying oven C is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven C is evacuated and a heating program is started; when the vacuum degree of the drying oven C reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on a weighing pan for heating; the heating is continued for a period of time, nitrogen is introduced into the drying oven C until the air pressure in the drying oven C is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed;

[0071] Repeat this process and regularly weigh the weighing bottle in the drying oven C until it reaches a constant weight.

[0072] When the weighing bottle in the drying oven C is heated for ≥6 hours, the sealing and heat-insulating device is opened, the weighing bottle is covered and moved into the third normal-temperature dryer for cooling to room temperature.

[0073] In an exemplary embodiment, step 4) includes: inputting the calculation formula into the analysis-transmission-storage device in advance, and after the test is completed, inputting the test results into the analysis-transmission-storage device to analyze and summarize the test results and determine the phase composition of the gypsum clinker.

[0074] Compared with the related art in the field, the present application has the following beneficial effects:

[0075] 1. The testing system and method for the phase composition of gypsum clinker described in the present application can effectively reduce the source of test errors, making the test results more accurate;

[0076] 2. The testing system and method for the phase composition of gypsum clinker described in this application can be used for rapid testing;

[0077] 3. The testing system and method for the phase composition of gypsum clinker described in this application can realize simultaneous analysis and testing of multiple groups of samples;

[0078] 4. The testing system and method for the phase composition of gypsum clinker described in the present application can summarize, compare and analyze the test results of multiple groups of samples, effectively reducing the operating errors and workload of laboratory operators.

[0079] Other features and advantages of the present application will be described in the following description, and partly become apparent from the description, or be understood by implementing the present application. Other advantages of the present application can be realized and obtained by the schemes described in the description and the drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0080] The accompanying drawings are used to provide an understanding of the technical solution of the present application and constitute a part of the specification. Together with the embodiments of the present application, they are used to explain the technical solution of the present application and do not constitute a limitation on the technical solution of the present application.

[0081] Figure 1 to Figure 2 This is a structural diagram of the testing system for the phase composition of gypsum clinker in this application.

[0082] Description of reference numerals:

[0083] 1-connection port; 2-sampling storage device; 3-drying box; 4-weighing device; 5-first sample transport pipeline; 6-second sample transport pipeline; 7-third sample transport pipeline; 8-sampler; 9-hanging table; 10-sample storage device; 11-sample storage table. DETAILED DESCRIPTION

[0084] The present invention is further described in detail below in conjunction with the embodiments, but the present invention is not limited thereto. Any equivalent substitutions in the field of interest made according to the disclosure of the present invention shall fall within the protection scope of the present invention.

[0085] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0086] In addition, the terms "first", "second", etc. are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first", "second", etc. may explicitly or implicitly include at least one of the features.

[0087] In the description of the present application, “plurality” means at least two, for example, two, three, etc., unless otherwise clearly and specifically defined.

[0088] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0089] In the present application, unless otherwise clearly specified and limited, a first feature being “above” or “below” a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being “above”, “top”, or “above” a second feature may mean that the first feature is directly at the top or obliquely at the top of the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being “below”, “below”, or “below” a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0090] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example" or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.

[0091] Example 1.

[0092] The testing system for the phase composition of gypsum clinker includes: a sampling device, one or more testing devices and an analysis-transmission-storage device; wherein one end of the sampling device is vacuum-connected to the gypsum production line to achieve real-time sampling; the other end is connected to the one or more testing devices via one or more sample transport pipelines to ensure that the samples can be transported to the testing devices according to the test requirements; the analysis-transmission-storage device is configured to analyze and summarize the test results during and after the test to determine the phase composition of the gypsum clinker.

[0093] The analysis-transmission-storage device includes a computer, and the sampling device and the testing device are respectively connected to the analysis-transmission-storage device, and are used to control the sampling device and the testing device to perform sampling and measurement respectively, so as to realize simultaneous online analysis and testing of multiple samples, and summarize, store and feedback the test results.

[0094] The sampling device is vacuum-connected to the gypsum production line through a vacuum pump. The sampling device comprises: a connection port 1, used to connect the sampling device to the gypsum production line; a sampling holder 2, the sampling holder 2 is connected to the connection port 1, used to achieve the retention and preservation of the sample, and a connecting pipe, the connecting pipe is used to connect the connection port 1 and the sampling holder 2. Among them, a sealing device is provided at the front end of the connecting pipe, which is used to seal the connection between the connection port and the gypsum production line, or the part where sampling is required; the vacuum pump is connected to the side of the connecting pipe.

[0095] The sampling storage device also includes a program control system; a vacuum control device and a temperature and humidity control device, which are used to control the vacuum degree and temperature and humidity in the sampling storage device to store the sample under vacuum temperature and humidity control.

[0096] like Figure 2As shown, the sampling preserver 2 is provided with a sampler 8, a hanging table 9, a sampling channel (not shown), a sampler 10 and a sampler table 11. The hanging table 9 is arranged on the front baffle of the sampling preserver 2 and is located at the upper part of the interface between the connecting pipe and the sampling preserver 2; the sampler 8 is hung on the hanging table 9; the sampling channel connects the sampler 8 and the interface; the sampler table 11 is arranged at the rear baffle of the sampling preserver 2, and the sampler 10 is placed on the sampler table 11 to complete the storage and numbering of the samples to be tested. Among them, the sampler 8 is a sampling cavity that can be opened and closed on both sides, including: a telescopic arm connected to the hanging table, a sampling spoon located in the sampler, and a spring connected to the sampling spoon. A translation device (not shown) can be arranged at the bottom of the sampler table 11, and the sampler table 11 translates between the sampler 8 and the rear baffle through the translation device.

[0097] like Figure 2 As shown, the sampling holder 2 includes a plurality of sample storage tables 11 arranged in parallel, and one or more sample storage containers 10 can be placed on the sample storage tables 11 .

[0098] The program control system in the sampling holder 2 can control: the telescopic arm sends the sampler 8 to the interface, the opening and closing of the sampling cavity, the movement of the sample storage table 11, and the linkage between the sampling holder 2 and the testing device.

[0099] like Figure 1 As shown, the sampling holder 2 is connected to the testing device via one or more sample transport pipes.

[0100] like Figure 1 As shown, the test device is a drying test device, which includes a drying box 3 and one or more weighing devices 4, wherein the weighing devices 4 are located at the top of the outer side of the drying box 3 and are thermally insulated from the drying box 3; specifically, the weighing device 4 is provided with a hanging rod and a placing device, and a through hole for accommodating the hanging rod to pass through is provided at the top of the drying box 3, and the placing device is suspended on the hanging rod and suspended in the drying box 3 for weighing the sample.

[0101] like Figure 1 As shown, the sample placing device is a weighing pan or a weighing bottle located on the weighing pan.

[0102] In this embodiment, the number of the sample transport pipeline and the number of the test device are 3, and the drying ovens corresponding to each of the test devices are drying oven A, drying oven B and drying oven C, which are used to measure the content of soluble type III anhydrous gypsum, hemihydrate gypsum and dihydrate gypsum respectively; each drying oven includes 6 weighing devices 4. In this embodiment, the drying temperature of the drying oven A is 230±3℃, the drying temperature of the drying oven B is 40±3℃, and the drying temperature of the drying oven C is 40±4℃; the vacuum degree of the drying oven A, the drying oven B and the drying oven C is -0.07MPa to -0.09MPa.

[0103] In this embodiment, the drying oven may also include a sample cleaning and processing device for cleaning and preserving samples after the test is completed.

[0104] Example 2.

[0105] In this embodiment, the method for analyzing the gypsum clinker phase composition using the testing system described in Example 1 is as follows:

[0106] 1) Connect the connection port 1 of the sampling device to the gypsum production line; specifically:

[0107] Before the connecting pipe of the sampling holder 2 is connected to the discharge port (or sampling port) of the gypsum production line, the connecting pipe is sealed first, and the vacuum pump is turned on to evacuate the connecting pipe, the sampling device, and the testing device; when the vacuum degree reaches -0.07MPa to -0.09MPa, the vacuuming is stopped, and the connecting pipe is connected to the discharge port (or sampling port) of the gypsum production line. After the connection is completed, the sealing device in the connecting pipe is opened to achieve communication, thereby realizing the overall connection between the sampling device and the gypsum production line;

[0108] 2) Sampling and preservation: The sampling device samples and preserves the gypsum clinker samples in the gypsum production line; specifically:

[0109] During sampling, the program control system controls the telescopic arm to send the sampler 8 to the interface between the connecting pipe and the sampling holder 2 through the sampling channel. At this time, the side of the sampler 8 adjacent to the interface is opened, and the spring in the sampling holder 2 ejects the sampling spoon in the sampler 8 to the discharge port (or sampling port) for sampling; after sampling, the spring contracts to retract the sampling spoon into the sampler 8. At this time, the side of the sampler 8 adjacent to the interface is closed, and the telescopic arm retracts the sampler 8 onto the hanging table 9 to complete the sampling;

[0110] When storing samples, the program control system controls the translation device at the bottom of the sample storage table 11 to translate the sample storage table 11 to the sampler 8, the sampler 8 is opened on the side adjacent to the sample storage table, the spring ejects the sampling spoon and places the sample in the sampler 10, then the spring contracts to retract the sampling spoon into the sampler 8, at this time, the sampler 8 is closed on the side adjacent to the sample storage table 11, the translation device translates the sample storage table 11 to the rear baffle of the sampling holder 2, the sample is stored, and sealed and stored at a reduced temperature;

[0111] 3) Testing: regularly transporting the gypsum clinker samples from the sampling device to one or more testing devices through one or more sample transport pipelines, and performing simultaneous drying and weighing tests on the multiple gypsum clinker samples in the testing devices; specifically:

[0112] When the test program is started, the test device completes all preparatory work before the test, including: evacuating the drying box and repeatedly weighing until the sample placement device reaches a constant weight;

[0113] The sample in the sample storage 10 is transported to the sample placing device in the weighing device through the sample transport pipeline;

[0114] The drying box of the test device is evacuated and the heating program is started. After the vacuum degree of the drying box reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and heating is continued for a period of time. Nitrogen is introduced into the drying box until the air pressure in the drying box is the same as the external atmospheric pressure, and the total weight of the placement device is weighed; wherein the continuous heating time is 0.5h or 1h;

[0115] Repeat this process, and weigh the sample placement device periodically until it reaches a constant weight, and then complete the test; wherein, when the difference between two weighings is no more than 0.5 g, the constant weight is reached;

[0116] 4) Displaying the results: The calculation formula is input into the analysis-transmission-storage device in advance. After the test is completed, the test results are analyzed and summarized by the analysis-transmission-storage device to determine the phase composition of the gypsum clinker.

[0117] Example 3.

[0118] On the basis of Example 2, the determination of the drying oven B in step 3) further includes:

[0119] The drying box B is connected to a first liquid storage cylinder containing 95% ethanol solution, and the drying box B is also connected to a second normal temperature dryer. Sealing and heat insulation devices are respectively provided between the drying box B and the first liquid storage cylinder and the second normal temperature dryer;

[0120] Slowly add 95% ethanol solution along the edge of the weighing bottle in the drying oven B, shake gently to make the sample in the drying oven B evenly moistened and let it stand;

[0121] The weighing bottle in the drying oven B is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven B is evacuated and the heating program is started; after the vacuum degree of the drying oven B reaches the working condition and the temperature reaches the set value, the evacuation is stopped, the bottle cap is opened and placed on a weighing pan for heating, and the heating is continued for a period of time, nitrogen is introduced into the drying oven B until the air pressure in the drying oven B is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed;

[0122] Repeat this process and regularly weigh the weighing bottle in the drying oven B until it reaches a constant weight.

[0123] When the weighing bottle in the drying oven B is heated for ≥6h, the weighing bottle is covered, the sealing and heat-insulating device is opened, and the weighing bottle is moved into the second normal-temperature dryer for cooling to room temperature;

[0124] Specifically, the test steps for the drying oven B are:

[0125] ① Weigh the empty weighing bottle m01 that has been dried to constant weight;

[0126] ② Weigh about 5g of the sample into a weighing bottle, accurate to 0.0001g, and record the mass m1;

[0127] ③ Slowly add about 5 ml of 95% ethanol solution along the edge of the weighing bottle, gently shake to make the sample evenly wet, and let it stand for 10 minutes;

[0128] ④Evacuate the drying oven and start the heating program to raise the temperature to (40±3)℃;

[0129] ⑤ Place the weighing bottle with the lid open on the weighing pan to heat;

[0130] ⑥Weigh the weighing bottle regularly. When the difference between two weighings with an interval of 1 hour is no more than 0.5 mg, it is a constant weight. Record the mass m4.

[0131] Example 4.

[0132] Based on Example 2, the determination of the drying oven C in step 3) includes the following steps:

[0133] The drying box C is connected to a second liquid storage cylinder containing distilled water, and the drying box C is also connected to a third normal temperature dryer. Sealing and heat insulation devices are respectively provided between the drying box C and the second liquid storage cylinder and the third normal temperature dryer;

[0134] Slowly add distilled water along the edge of the weighing bottle of the drying oven C, and shake gently to make the sample in the drying oven C evenly moistened and soaked;

[0135] The weighing bottle in the drying oven C is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven C is evacuated and a heating program is started; when the vacuum degree of the drying oven C reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on a weighing pan for heating; the heating is continued for a period of time, nitrogen is introduced into the drying oven C until the air pressure in the drying oven C is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed;

[0136] Repeat this process and regularly weigh the weighing bottle in the drying oven C until it reaches a constant weight.

[0137] When the weighing bottle in the drying oven C is heated for ≥6h, the sealing and heat-insulating device is opened, the weighing bottle is covered and moved into the third normal temperature dryer for cooling to room temperature;

[0138] Specifically, the test steps for the drying oven C are:

[0139] ① Weigh the empty weighing bottle m02 that has been dried to constant weight;

[0140] ② Weigh about 2g of sample into a weighing bottle, accurate to 0.0001g, and record the mass m3;

[0141] ③ Slowly add about 2 ml of distilled water along the edge of the weighing bottle, gently shake to make the sample evenly moistened, and soak for 2 hours;

[0142] ④Evacuate the drying oven and start the heating program to raise the temperature to (40±4)℃;

[0143] ⑤Open the lid of the weighing bottle and place the lid on the weighing pan;

[0144] ⑥Weigh the weighing bottle regularly. When the difference between two weighings with an interval of 1 hour is no more than 0.5 mg, it is a constant weight. Record the mass m2.

[0145] Example 5.

[0146] On the basis of Example 2, the determination of the drying oven A in step 3) further includes:

[0147] The drying box A is connected to a first normal temperature dryer, and a sealing and heat-insulating device is provided between the drying box A and the first normal temperature dryer;

[0148] The weighing bottle in the drying oven A is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven A is evacuated and the heating program is started; when the vacuum degree of the drying oven A reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on the weighing pan; heating is continued for a period of time, nitrogen is introduced into the drying oven A until the air pressure in the drying oven A is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed;

[0149] Repeat this process and regularly weigh the weighing bottle in the drying oven A until it reaches a constant weight.

[0150] When the heating is completed, the sealed heat-insulating device is opened, and the weighing bottle is transported to the first normal-temperature dryer for cooling;

[0151] Specifically, the test steps for the drying oven A are:

[0152] ① Weigh the empty weighing bottle m03 that has been dried to constant weight;

[0153] ② Weigh about 5g of the sample into a weighing bottle, accurate to 0.0001g, and record the mass m5;

[0154] ③Evacuate the drying oven and start the heating program to raise the temperature to (230±3)℃;

[0155] ④Open the lid of the weighing bottle and place the lid of the weighing bottle on the weighing pan; heat for 120 minutes;

[0156] ⑤ Immediately cover the weighing bottle with a lid (but not too tightly), place it in the first normal temperature dryer to cool for 30 minutes, cover it tightly with a lid, and weigh it;

[0157] ⑥ Move the weighing bottle into drying oven A and heat it for 0.5h again. Cool it according to step ⑤ and weigh the weighing bottle. Repeat this process. When the difference between two weighings with a heating time interval of 0.5h is no more than 0.5mg, the weight is constant. Record the mass m6.

[0158] Example 6.

[0159] In Examples 3-5, the calculation formulas in the drying ovens A, B, and C are as follows:

[0160] When m1>m2, the adhering water content is expressed in mass fraction W. a1 According to formula (1), the content of soluble anhydrite (AⅢ) is W A1 =0;

[0161]

[0162] Where:

[0163] w a1------Mass fraction of attached water in the sample;

[0164] m 01 ------Mass of the empty weighing bottle, in grams (g);

[0165] m1------The mass of (weighing bottle + sample) before adding ethanol solution, in grams (g);

[0166] m2------The mass of the weighing bottle + sample after adding ethanol solution and drying to constant weight, in grams (g);

[0167] When m1<m2, soluble anhydrous gypsum (A Ⅲ ) content in mass fraction w A1 According to formula (2), the adhering water content w a1 =0;

[0168]

[0169] Where:

[0170] w A1 ------Soluble anhydrous gypsum (A Ⅲ )’s mass fraction;

[0171] m 01 ------Mass of the empty weighing bottle, in grams (g);

[0172] m1------The mass of (weighing bottle + sample) before adding ethanol solution, in grams (g);

[0173] m2------The mass of the weighing bottle + sample after adding ethanol solution and drying to constant weight, in grams (g); the mass change of the sample after hydration is calculated as mass fraction c1 according to formula (3)

[0174]

[0175] Where:

[0176] c1------mass change fraction of the sample after hydration;

[0177] m 02 ------Mass of the empty weighing bottle, in grams (g);

[0178] m3------The mass of (weighing bottle + sample) before adding water, in grams (g)

[0179] m4------The mass of the weighing bottle + sample after adding water and drying to constant weight, in grams (g);

[0180] The content of hemihydrate gypsum (HH) is calculated by mass fraction w HH1 as follows:

[0181] When m1 > m2: Calculate according to formula (4):

[0182] w HH1 = 5.37×(c1 + w a1 )×100% (4)

[0183] In the formula:

[0184] w HH1 ------ Mass fraction of hemihydrate gypsum (HH) in the sample;

[0185] c1 ------ Mass change fraction after hydration of the sample;

[0186] w a1 ------ Mass fraction of adsorbed water in the sample;

[0187] When m1 < m2, calculate according to formula (5):

[0188] w HH1 = 5.37×(c1 - 0.265×w A1 )×100% (5)

[0189] In the formula:

[0190] w HH1 ------ Mass fraction of hemihydrate gypsum (HH) in the sample;

[0191] c1 ------ Mass change fraction after hydration of the sample;

[0192] w A1 ------ Mass fraction of soluble anhydrite (AⅢ) in the sample.

[0193] The mass change of the sample during heating is calculated by mass fraction d1 according to formula (6).

[0194]

[0195] In the formula:

[0196] d1 ------ Mass change fraction of the sample during heating;

[0197] m 03 ------ Mass of the empty weighing bottle, unit: gram (g);

[0198] m5 ------ Mass of (weighing bottle + sample) before heating, unit: gram (g);

[0199] m6------The mass of the weighing bottle + sample after drying to constant weight, in grams (g).

[0200] The content of dihydrate gypsum (DH) is expressed as mass fraction w DH1 The calculation method is as follows:

[0201] When m1>m2: Calculate according to formula (7):

[0202] w DH1 =4.78×[(d1-w a1 )-0.062×w HH1 ]×100% (7)

[0203] Where:

[0204] w DH1 ------Mass fraction of dihydrate gypsum (DH) in the sample;

[0205] d1------The fraction of mass change of the sample during heating;

[0206] w a1 ------Mass fraction of attached water in the sample;

[0207] w HH1 ------Mass fraction of hemihydrate gypsum (HH) in the sample.

[0208] When m1<m2, calculate according to formula (8):

[0209] w DH1 =4.78×(d1-0.062×w HH1 )×100% (8)

[0210] Where:

[0211] w DH1 ------Mass fraction of dihydrate gypsum (DH) in the sample;

[0212] d1------The fraction of mass change of the sample during heating;

[0213] w HH1 ------Mass fraction of hemihydrate gypsum (HH) in the sample.

[0214] Examples 7-12.

[0215] The test system and method in Examples 1-6 were used to perform the analysis. The results are shown in Table 1.

[0216] In Example 7, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 230°C, 43°C and 44°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.08MPa.

[0217] In Example 8, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 230°C, 40°C and 40°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.085MPa.

[0218] In Example 9, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 233°C, 43°C and 44°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.08MPa.

[0219] In Example 10, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 230°C, 37°C and 36°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.08MPa.

[0220] In Example 11, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 230°C, 37°C and 36°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.085MPa.

[0221] In Example 12, the drying temperatures of the drying oven A, the drying oven B and the drying oven C can be set to 227°C, 40°C and 40°C respectively; at the same time, the drying ovens can also be evacuated, wherein the vacuum degree in the drying ovens A, B and C can be -0.085MPa.

[0222] Test example:

[0223] The values ​​measured in Examples 7-12 were compared with the values ​​measured by the conventional oven method and thermal analyzer method, and the results are shown in Table 1. The oven method and thermal analyzer method test methods refer to the National Standard of the People's Republic of China GB / T36141-2018 "Analysis Method for Phase Composition of Building Gypsum".

[0224] Table 1

[0225]

[0226] According to Table 1, compared with the oven method and the thermal analyzer method, the testing system and method for the phase composition of gypsum clinker described in the present application can effectively reduce the source of test errors, make the test results more accurate, enable rapid testing, and achieve simultaneous analysis and testing of multiple groups of samples. The test results of multiple groups of samples can be summarized, compared and analyzed, effectively reducing the workload of laboratory operators.

[0227] Although the embodiments of the present application have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be understood as limitations on the present application. Ordinary technicians in this field can change, modify, replace and modify the above embodiments within the scope of the present application.

Claims

1. A testing system for gypsum clinker phase composition, comprising: a sampling device, one or more test devices, and an analysis-transmission-storage device; Wherein, one end of the sampling device is connected to the gypsum production line, and the other end is connected to the one or more testing devices through one or more sample transport pipelines; The analysis-transmission-storage device is configured to analyze and summarize the test results during and after the test to determine the phase composition of the gypsum clinker.

2. The testing system for the phase composition of gypsum clinker according to claim 1, wherein: The sampling device is vacuum-connected to the gypsum production line via a vacuum pump.

3. The testing system for the phase composition of gypsum clinker according to claim 2, wherein: The sampling device comprises: A connection port, used to connect the sampling device to a gypsum production line; A sampling holder connected to the connection port; A connecting pipe, wherein the connecting pipe connects the connection port and the sampling storage container; Optionally, a sealing device is provided at the front end of the connecting pipe, which is used to seal the connection port with the connection of the gypsum production line or the part where sampling is required; the vacuum pump is connected to the side of the connecting pipe; Optionally, the sampling storage container is also provided with a program control system, a vacuum control device and a temperature and humidity control device.

4. The testing system for the phase composition of gypsum clinker according to claim 3, wherein: The sampling and preserving device comprises: a hanging platform, a sampling channel, a sampler, a sample storage device and a sample storage platform; the hanging platform is arranged on a front baffle in the sampling and preserving device and is located at the upper part of the interface between the connecting pipe and the sampling and preserving device; the sampler is hung on the hanging platform, and the sampling channel is connected to the sampler and the interface; the sample storage platform is arranged on a rear baffle in the sampling and preserving device, and the sample storage device is located on the sample storage platform; Optionally, the sampler is a sampling cavity capable of opening and closing on both sides, comprising: a telescopic arm connected to the hanging platform, a sampling spoon located in the sampler, and a spring connected to the sampling spoon; Optionally, a translation device may be provided at the bottom of the sample storage table; the sample storage table translates between the sampler and the rear baffle through the translation device; Optionally, one or more sample storage devices are placed on the sample storage table; Optionally, a plurality of parallel sample storage tables are provided in the sampling storage container; Optionally, the sampling holder is connected to the testing device via one or more sample transport pipes.

5. The testing system for the phase composition of gypsum clinker according to any one of claims 1 to 4, wherein: The test device is a drying test device, comprising a drying box and one or more weighing devices; the weighing devices are located on the top of the outer side of the drying box and are thermally insulated from the drying box; Optionally, the weighing device is provided with a suspension rod and a sample placing device, the top of the drying box is provided with a through hole for accommodating the suspension rod to pass through, and the sample placing device is suspended on the suspension rod and suspended in the drying box; Optionally, the sample placing device is a weighing pan or a weighing bottle located on the weighing pan.

6. The testing system for the phase composition of gypsum clinker according to claim 5, wherein: The drying temperature of the drying oven is 40-45°C or 220-240°C; and / or The vacuum degree of the drying oven is -0.07MPa to -0.09MPa; and / or The number of the testing devices is 3; the number of the weighing devices in each of the testing devices is 6; and / or The drying box also includes a sample cleaning and processing device.

7. A method for testing the phase composition of gypsum clinker, the method using the testing device for the phase composition of gypsum clinker according to any one of claims 1 to 6 for determination, the method comprising the following steps: 1) connecting the sampling device to a gypsum production line; 2) Sampling and preservation: the sampling device samples and preserves the gypsum clinker samples in the gypsum production line; 3) Testing: regularly transporting the gypsum clinker sample from the sampling device to the one or more testing devices through the one or more sample transport pipes; Performing simultaneous drying and weighing tests on a plurality of gypsum clinker samples in the testing device; 4) Displaying the results: the calculation formula is input into the analysis-transmission-storage device in advance. After the test is completed, the test results are analyzed and summarized by the analysis-transmission-storage device to determine the phase composition of the gypsum clinker.

8. The method according to claim 7, wherein: Step 1) includes: Before connecting the connecting pipe of the sampling preserver to the discharge port or sampling port of the gypsum production line, the connecting pipe is first sealed, and the vacuum pump is turned on to evacuate the connecting pipe, the sampling device, and the testing device; when the vacuum degree reaches the working condition, the vacuuming is stopped, and the sealed connecting pipe is connected and communicated with the discharge port or sampling port of the gypsum production line; Optionally, the vacuum degree of the vacuum pump is -0.07 MPa to -0.09 MPa.

9. The method according to claim 8, wherein: Step 2) includes: when sampling, the program control system controls the telescopic arm to send the sampler to the interface between the connecting pipe and the sampling holder through the sampling channel, at this time, the side of the sampler adjacent to the interface is opened, and the spring in the sampling holder ejects the sampling key in the sampler to the discharge port or sampling port for sampling; after sampling, the spring contracts to recycle the sampling key into the sampler, at this time, the side of the sampler adjacent to the interface is closed, and the telescopic arm recycles the sampler to the hanging table to complete the sampling; When storing samples, the program control system controls the translation device at the bottom of the sample storage table to translate the sample storage table to the sampler, and the sampler opens on a side adjacent to the sample storage table. The spring pops out the sampling spoon and places the sample in the sample storage of the sample storage table. Subsequently, the spring contracts to retract the sampling spoon into the sampler. At this time, the sampler closes on a side adjacent to the sample storage table, and the translation device translates the sample storage table to the rear baffle of the sampling storage device to complete the storage of the sample, and seals and cools it down.

10. The method according to claim 9, wherein: Step 3) includes: When the test program is started, the test device completes all preparatory work before the test; Transporting the sample in the sample storage device to the sample placing device in the weighing device through the sample transport pipeline; The drying box is evacuated and a heating program is started, and the evacuation is stopped when the vacuum degree of the drying box reaches the working condition and the temperature reaches the set value; the heating is continued for a period of time, and nitrogen is introduced into the drying box until the air pressure in the drying box is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed; Repeat this process, and weigh the sample placing device periodically until it reaches a constant weight, and then complete the test; Optionally, the preparatory work before the test includes: evacuating the drying box and repeatedly weighing until the sample placement device reaches a constant weight; Optionally, the heating time is 0.5h or 1h; Optionally, constant weight is achieved when the difference between two weighings with a heating time interval of 0.5 h or 1 h is no more than 0.5 g.

11. The method according to any one of claims 7 to 10, wherein: The drying ovens in the test device are drying oven A, drying oven B and drying oven C; Optionally, the drying temperature of the drying oven A is 230±3°C, the drying temperature of the drying oven B is 40±3°C, and the drying temperature of the drying oven C is 40±4°C.

12. The method according to claim 11, wherein: When the drying oven is the drying oven A, step 3) further comprises: The drying box A is connected to a first normal temperature dryer, and a sealing and heat-insulating device is provided between the drying box A and the first normal temperature dryer; The weighing bottle in the drying oven A is covered with a bottle cap, the sealing and heat-insulating device is closed, and the drying oven A is evacuated and a heating program is started; When the vacuum degree of the drying oven A reaches the working condition and the temperature reaches the set value, stop the vacuuming, open the bottle cap and place it on the weighing pan for heating; continue heating for a period of time, introduce nitrogen into the drying oven A until the air pressure in the drying oven A is the same as the external atmospheric pressure, and weigh the total weight of the sample placement device; Repeat this process and regularly weigh the weighing bottle in the drying oven A until it reaches a constant weight; When the heating is completed, the sealed heat-insulating device is opened, and the weighing bottle is transported to the first normal-temperature dryer for cooling.

13. The method according to claim 11, wherein: When the drying oven is the drying oven B, step 3) further comprises: The drying box B is connected to a first liquid storage cylinder containing 95% ethanol solution, and the drying box B is also connected to a second normal temperature dryer. Sealing and heat insulation devices are respectively provided between the drying box B and the first liquid storage cylinder and the second normal temperature dryer; Slowly add 95% ethanol solution along the edge of the weighing bottle in the drying oven B, shake gently to make the sample in the drying oven B evenly moistened and let it stand; The weighing bottle in the drying oven B is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven B is evacuated and a heating program is started; when the vacuum degree of the drying oven B reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on a weighing pan for heating; the heating is continued for a period of time, nitrogen is introduced into the drying oven B until the air pressure in the drying oven B is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed; Repeat this process and regularly weigh the weighing bottle in the drying oven B until it reaches a constant weight; When the weighing bottle in the drying box B is heated for ≥6 hours, the sealing and heat-insulating device is opened, the bottle cap is covered, and the weighing bottle is moved into the second normal-temperature dryer for cooling to room temperature.

14. The method according to claim 11, wherein: When the drying oven is the drying oven C, step 3) further comprises: The drying box C is connected to a second liquid storage cylinder containing distilled water, and the drying box C is also connected to a third normal temperature dryer. Sealing and heat insulation devices are respectively provided between the drying box C and the second liquid storage cylinder and the third normal temperature dryer; Slowly add distilled water along the edge of the weighing bottle of the drying oven C, and shake gently to make the sample in the drying oven C evenly moistened and soaked; The weighing bottle in the drying oven C is covered with a bottle cap, the sealing and heat-insulating device is closed, the drying oven C is evacuated and a heating program is started; when the vacuum degree of the drying oven C reaches the working condition and the temperature reaches the set value, the evacuation is stopped, and the bottle cap is opened and placed on a weighing pan for heating; the heating is continued for a period of time, nitrogen is introduced into the drying oven C until the air pressure in the drying oven C is the same as the external atmospheric pressure, and the total weight of the sample placement device is weighed; Repeat this process and regularly weigh the weighing bottle in the drying oven C until it reaches a constant weight. When the weighing bottle in the drying oven C is heated for ≥6 hours, the sealing and heat-insulating device is opened, the bottle cap is covered, and the weighing bottle is moved into the third normal-temperature dryer for cooling to room temperature.

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