Device and method for rapidly measuring water loss rate of freeze-dried butyl rubber plug under simple condition
By designing a quick measurement device for water loss rate of simple freeze-dried butyl rubber plugs, using oven drying weighing method and sealing protrusions, the problems of long-term water loss rate test and large measurement errors are solved, and rapid and accurate water loss is achieved rate measurement.
Patent Information
- Application Number
- CN202411383482.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2025-01-03
AI Technical Summary
The general weighing method takes a long time to perform water loss test and the measurement error is large after cooling.
A rapid measurement device for water loss rate of lyophilized butyl rubber plugs under simple conditions is designed, including a cylindrical hollow structure and sealing protrusions that can be assembled. It is prepared by ABS material and 3D printing, combined with oven drying and weighing method to reduce Cooling time and improve sealing through sealing projections and sealing tapes, simplifying operation.
It greatly shortens the experimental time of conventional oven drying methods, improves measurement efficiency, reduces equipment requirements, and ensures the accuracy and simplicity of measurement.
Smart Images
Figure CN119246321A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of analytical measuring devices, in particular to a device and method for quickly measuring the water loss rate of a freeze-dried butyl rubber plug under simple conditions. Background Art
[0002] The key evaluation indicators of the performance of freeze-dried butyl rubber stoppers include moisture content, puncture force and puncture debris, tightness and self-sealing, insoluble particles, chemical stability, anti-freezing performance, etc. At the same time, the production and quality control of rubber stoppers should follow relevant pharmacopoeias or industry standards to ensure their safety and effectiveness. Among them, moisture content is crucial. The main reason is that the moisture in the product is removed during the freeze-drying process to improve its long-term storage stability. If the moisture content in the freeze-dried rubber stopper is too high, it may cause the freeze-dried product to re-absorb moisture, decompose or deteriorate, affecting the efficacy and safety of the drug. Second: If the moisture content in the freeze-dried rubber stopper is too high, it may promote the growth of microorganisms, thereby contaminating the freeze-dried product and affecting its safety. Third: Moisture may promote chemical reactions in freeze-dried products, resulting in decreased product performance. In summary, controlling the moisture content of freeze-dried rubber stoppers is crucial to ensuring the safety, stability, effectiveness and quality of freeze-dried products.
[0003] The water loss rate test is generally to repeatedly measure the mass of a certain amount of pre-treated rubber stoppers under certain drying conditions, and obtain a continuous and gradually decreasing quality curve that finally remains stable. A set of water change data of the rubber stoppers under this condition is calculated by the water loss rate formula. In the early stage of formula development, the water loss rate experimental data of freeze-dried butyl rubber stoppers is an important basis for evaluating the feasibility of the formula. Rubber stoppers with different formulas will affect the moisture change of freeze-dried products during the stability period. For example, the residual moisture measured for halogenated rubber stoppers is different from that for non-halogenated rubber stoppers. The water loss rate test can help evaluate the water release of rubber stoppers during the freeze-drying process. By testing the water loss rate of rubber stoppers under different conditions, the best drying and processing methods can be determined to improve the performance of freeze-dried rubber stoppers.
[0004] Common methods for measuring the moisture content of rubber stoppers include: Karl Fischer method, infrared spectroscopy, rapid moisture meter method, and oven drying weighing method. The principle of Karl Fischer method is to measure the moisture content in liquids, solids and gases through chemical reactions. It has high accuracy and strong specificity, but the operation is complicated. Infrared spectroscopy uses the absorption characteristics of water molecules to infrared of a specific wavelength to measure moisture. It is fast and non-destructive, but may be interfered by other substances. The rapid moisture meter method is based on the oven drying weight loss method. It uses efficient heating elements and a precise weighing system to automatically calculate the moisture content. It is simple to operate and has a fast measurement speed, but too high a heating temperature may cause other substances inside the rubber stopper to volatilize and cause errors. The above three test methods all have specific requirements for experimental equipment, and some methods also test the high experimental literacy of the operator. Therefore, in comparison, the oven drying weighing method is the most universal and has a higher accuracy rate. The instruments used only require a general electric blast drying oven and a general electronic balance.
[0005] However, the general weighing method takes too long to test the water loss rate, that is, the oven drying time plus the time the container needs to cool to room temperature before each weighing. Cooling to room temperature is to balance the internal and external temperatures, avoid measurement errors caused by temperature differences, and ensure that the measured value of moisture content is more reliable, but storage at room temperature will rebalance the moisture inside the rubber stopper. This device uses a simple oven and a balance as test instruments, supplemented by a closed fixture, and weighs the container together, thereby reducing the cooling time and greatly improving the test efficiency. At the same time, this test method has low requirements for testing equipment and is universal. Summary of the invention
[0006] The technical problem to be solved by the present invention is that the water loss rate test using the general weighing method takes a long time and has a large measurement error after cooling.
[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is: a device for quickly measuring the water loss rate of freeze-dried butyl rubber stoppers under simple conditions, comprising a left frame and a right frame that can be assembled to form a cylindrical hollow structure, one opposite end of the left frame and the right frame is connected by a hinge, and the assembled end faces of the left frame and the right frame are respectively provided with a sealing protrusion and a sealing groove for inserting the sealing protrusion, and the left frame and the right frame are respectively connected with a left handle and a right handle.
[0008] Preferably, a torsion spring is mounted on the hinge shaft, two ends of the torsion spring are respectively connected to the left frame and the right frame, and the torsion spring is in a pulled apart state when the left frame and the right frame are in a spliced state.
[0009] Preferably, a sealing belt is provided on the outer side of the sealing protrusion.
[0010] Preferably, the measuring device as a whole is made of ABS as a base material and is prepared by 3D printing.
[0011] A method for quickly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions, characterized in that it comprises the following steps: Step 1: Pretreatment: weigh the freeze-dried rubber plug, heat it in a small beaker, perform moist heat sterilization, then place the small beaker in a measuring device for weighing, and use the weight as the first set of data; Step 2, experimental process, set the oven drying conditions, take out the small beaker in the measuring device, and place it in the oven for multiple heating. After each heating, place the small beaker in the measuring device for weighing and record the weight data; Step 3: Data processing, moisture calculation formula is: , where m1 is the net weight of the rubber plug before sterilization, and m2 is the net weight of the rubber plug after drying. The water loss rate graph of the movable rod rubber plug is drawn according to the obtained data, and finally the test result of the water loss rate of the movable rod rubber plug under dry conditions is obtained.
[0012] Preferably, in step 1, the top of the small beaker is first sealed with tin foil, and then holes are punched in the tin foil, and the tin foil is removed before the small beaker enters the oven.
[0013] Preferably, in step 2, the drying temperature is set to 105° C., the drying time is 30 minutes each time, and seven groups of drying tests are repeated.
[0014] 1. The present invention provides a device and method for quickly measuring the water loss rate of freeze-dried butyl rubber stoppers under simple conditions, which can greatly shorten the experimental time of the conventional oven drying method. The clamp used can be adjusted according to the required specifications and opening angles, and the internal material and insulation material can also be replaced according to the usage scenario.
[0015] 2. The measuring device and method have extremely low equipment requirements and are simple to operate, and can accurately and effectively evaluate the water loss rate of freeze-dried rubber plugs. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The present invention will be further described below in conjunction with the accompanying drawings and embodiments: Figure 1 It is a closed side view of an embodiment of the present invention.
[0017] Figure 2 This is an open rear view of an embodiment of the present invention.
[0018] Figure 3 It is an open side view of an embodiment of the present invention.
[0019] Figure 4 It is a top view of an opening of an embodiment of the present invention.
[0020] Figure 5 The rendering is used to simulate the embodiment of the present invention.
[0021] Figure 6 It is the water loss rate graph drawn in the embodiment of the present invention.
[0022] In the figure: 1, left side frame; 2, right side frame; 3, left side handle; 4, right side handle; 5, hinge shaft; 6, sealing protrusion. DETAILED DESCRIPTION
[0023] like Figure 1-5 As shown, the present invention provides a device for quickly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions, comprising a left side frame 1 and a right side frame 2 that can be assembled to form a cylindrical hollow structure, one opposite end of the left side frame 1 and the right side frame 2 are connected by a hinge shaft 5, and the assembled end surfaces of the left side frame 1 and the right side frame 2 are respectively provided with a sealing protrusion 6 and a sealing groove for inserting the sealing protrusion 6, and the left side frame 1 and the right side frame 2 are respectively connected with a left handle 3 and a right handle 4.
[0024] The whole measuring device can be realized by 3D printing technology to improve the integrity of the measuring device. The materials used are aluminum alloy, ABS (acrylonitrile-butadiene-styrene) or nylon materials with low density, good heat resistance and certain bearing capacity. Plastic injection molding technology can also be used to meet the requirements of complex shapes and precise sizes. PE (polyethylene), PVC (polyvinyl chloride) or general engineering plastics can be used. The internal materials need to use light and efficient heat-insulating materials, such as porous vacuum silicon, ceramic fiber paper and other new heat-resistant materials.
[0025] When the measuring device is opened, the movable ends of the left frame 1 and the right frame 2 can be moved away from each other by pressing the left handle 3 and the rear handle 4 together.
[0026] As a preferred embodiment of the present invention. The hinge shaft 5 is provided with a torsion spring, the two ends of which are respectively connected to the left frame 1 and the right frame 2, and the torsion spring is in a pulled apart state when the left frame 1 and the right frame 2 are in a spliced state. The torsion spring is used to limit the closing of the left frame 1 and the right frame 2, so that after the small beaker is placed in the measuring device, the staff releases the left handle 3 and the right handle 4, and the measuring device is automatically closed.
[0027] As a preferred embodiment of the present invention, a sealing belt is arranged outside the sealing protrusion 6. The sealing protrusion 6, the sealing groove and the sealing belt are arranged to ensure the sealing of the measuring device after closing, so as to reduce the moisture in the air from entering the measuring device and improve the accuracy of the water loss rate measurement.
[0028] A method for quickly measuring the water loss rate of freeze-dried butyl rubber stoppers under simple conditions comprises the following steps: Pretreatment: Take a conventional 30-40g freeze-dried rubber stopper and a small beaker for pretreatment with wet heat sterilization at 121℃ for 30 minutes. Cover the bottle mouth with a layer of perforated tin foil. This is to restore the moisture state of the rubber stopper before cleaning and drying as much as possible. Liquid water may exist, so it cannot be used as the weight before drying in the calculation formula. After this step, use a clamp to clamp and weigh, and use this weight as the first set of data. Weighing is required before operation, including the weight of the empty beaker, the clamp, and the beaker with the rubber stopper. The weight of the empty beaker, the weight of the empty measuring device, the weight of the beaker plus the rubber stopper, and the weight of the rubber stopper are shown in the following table:
[0029] Table showing the relationship between the total weight of beaker + measuring device + rubber stopper and moist heat sterilization time:
[0030] Experimental process: set the oven drying conditions to 105℃, 30 minutes (specific temperature and time can be adjusted), repeat the drying test seven times after preheating (the number of groups can also be adjusted according to the characteristics of the rubber stopper and the drying conditions), remove the tin foil and put the beaker into the oven. After each drying, use a clamp to move the beaker to the balance for weighing and record the relevant data, a total of nine groups.
[0031] Data processing: The moisture calculation formula is: , where m1 is the net weight of the rubber stopper before sterilization, and m2 is the net weight of the rubber stopper after drying. SPSS, Excel and other software were used to statistically analyze all the data and draw graphs to obtain the following Figure 6 The water loss rate curve shown in the figure can finally obtain the test result of the water loss rate of the freeze-dried rubber plug under the drying condition of 105°C.
[0032] Relationship table between drying time and water loss rate:
Claims
1. A device for quickly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions, characterized in that: The invention comprises a left side frame (1) and a right side frame (2) which can be assembled to form a cylindrical hollow structure. One opposite end of the left side frame (1) and the right side frame (2) are connected via a hinge shaft (5). The assembled end surfaces of the left side frame (1) and the right side frame (2) are respectively provided with a sealing protrusion (6) and a sealing groove for inserting the sealing protrusion (6). The left side frame (1) and the right side frame (2) are respectively connected with a left handle (3) and a right handle (4).
2. A device for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as claimed in claim 1, characterized in that: A torsion spring is sleeved on the hinge shaft (5), and two ends of the torsion spring are respectively connected to the left side frame (1) and the right side frame (2), and when the left side frame (1) and the right side frame (2) are in a spliced state, the torsion spring is in a pulled apart state.
3. A device for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as claimed in claim 1, characterized in that: A sealing belt is provided on the outer side of the sealing protrusion (6).
4. A device for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as claimed in claim 1, characterized in that: The measuring device as a whole is made of ABS as a base material and is prepared by 3D printing.
5. A method for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as described in any one of claims 1 to 4, characterized in that: The steps include: Step 1: Pretreatment: weigh the freeze-dried rubber plug, heat it in a small beaker, perform moist heat sterilization, then place the small beaker in a measuring device for weighing, and use the weight as the first set of data; Step 2, experimental process, set the oven drying conditions, take out the small beaker in the measuring device, and place it in the oven for multiple heating. After each heating, place the small beaker in the measuring device for weighing and record the weight data; Step 3: Data processing, moisture calculation formula is: , where m1 is the net weight of the rubber plug before sterilization, and m2 is the net weight of the rubber plug after drying. The water loss rate graph of the movable rod rubber plug is drawn according to the obtained data, and finally the test result of the water loss rate of the movable rod rubber plug under dry conditions is obtained.
6. A method for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as claimed in claim 5, characterized in that: In the step 1, the top of the small beaker is first sealed with tin foil, and then holes are punched in the tin foil, and the tin foil is removed before the small beaker enters the oven.
7. A method for rapidly measuring the water loss rate of freeze-dried butyl rubber plugs under simple conditions as claimed in claim 5, characterized in that: In step 2, the drying temperature is set to 105° C., the drying time is 30 minutes each time, and seven groups of drying tests are repeated.