CN210720215U - Full-automatic video melting point appearance - Google Patents
Full-automatic video melting point appearance Download PDFInfo
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- CN210720215U CN210720215U CN201921360602.2U CN201921360602U CN210720215U CN 210720215 U CN210720215 U CN 210720215U CN 201921360602 U CN201921360602 U CN 201921360602U CN 210720215 U CN210720215 U CN 210720215U
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Abstract
The utility model provides a full-automatic video melting point appearance, including heating module, video display unit, temperature control module, the glass capillary, light source and detector, a serial communication port, the metal indicator pole has been placed in the glass capillary, the cylinder of metal indicator pole lower part for long 5-15mm, there is the water conservancy diversion mouth all around the cylinder bottom, the water conservancy diversion mouth is connected with liquid sample storage area, a liquid water conservancy diversion to sample storage area after being used for will melting, be high 100 in metal indicator pole middle part for adding organic material 130 mm's cylinder, there is a light trap on this cylinder, it is continuous with the metal indicator pole to have the metal counter weight on metal indicator pole top, there is a height-adjustable's baffle between the glass capillary of light source and year appearance, there is an incident light hole on the baffle. The utility model provides a survey of easily changing look compound melting point, avoided the error that different year appearance volumes brought, simplified operation process guarantees the accuracy and the precision of testing result, has also expanded the range of application of full-automatic video melting point appearance simultaneously.
Description
Technical Field
The invention belongs to the technical field of analytical instruments, and particularly relates to a device and a method for measuring a melting point of a discolorable compound.
Background
Melting point refers to the temperature at which a crystalline material equilibrates between solid and liquid states, i.e., the temperature at which it changes from a solid to a liquid state. The cohesive force among molecules of the crystal substance and the properties of crystal lattice energy are factors influencing the melting point of the substance. According to the difference of structural particles and acting force, the crystals can be divided into molecular crystals, atomic crystals, ionic crystals, metal crystals and the like, and crystal substances are combined by ionic bonds, covalent bonds, metal bonds, hydrogen bonds and the like. When the crystal substance absorbs external energy, chemical bonds or intermolecular forces are broken to change the crystal substance from a solid state to a liquid state. The weaker the intermolecular force or the lower the bond energy of the chemical bond, the lower the melting point of the substance, and vice versa. Melting point is an important physical constant and is one of the important methods for determining purity. Therefore, melting point meters are widely used in chemical industry and medical research.
The photoelectric detector melting point instrument is widely applied in the market at present, and is continuously improved in use. CN 208060422U designs a drying bin and a grinding bin, and a magnetron in the drying bin heats the raw materials by microwaves to remove moisture in the raw materials, so that the test accuracy is improved; the milling motor at the top of the milling bin drives the milling roller to mill the raw materials, so that sample particles are smaller and more uniform, the contact area of hot air and materials in the heating process is increased, and the time required by testing is saved. Patent CN 101696948B has designed a no thermal hysteresis effect capillary melting point appearance with even temperature field, adopts liquid heating medium, electric heating, including heating system and temperature measurement system two parts, because the thermal hysteresis effect has been corrected through theoretical calculation for thermal hysteresis system error has been eliminated in the measurement of full melting point. The patent CN 202522530U adopts the photoelectric detection technique, can realize the automated inspection function, also has the function of artifical visual measurement, has improved the detection precision and the reliability of melting point, has enlarged detection sample scope, simple structure. Patent CN 203310785U has designed a video melting point appearance, and this melting point appearance can show temperature curve and real-time video image directly perceivedly to realized functions such as save, playback, shoot and record with video recording, accessible video observation color change and decomposition temperature have realized comprehensive integration heat preservation design, thereby make the measurement more stable more accurate, improved the ability of resisting external environment interference. Patent CN 205192243U has improved melting point appearance intensification subassembly structure, and it inlays the installation of piece formula with the capillary of heating part, during the maintenance, only need change the mold insert can, practiced thrift cost of maintenance. Patent CN 207007602U has designed a melting point appearance capillary system appearance device, and the device can guarantee the closely knit homogeneity of sample in the capillary to ensure the accuracy and the convenience of experiment, the effectual system appearance problem of melting point appearance capillary of having solved, and operation convenient to use. Patent CN 109444207A introduces a set of image recognition software for automatically determining the melting point of a compound, capturing the melting state of the compound at different time periods by a camera, feeding back the captured image information to a control system for analysis, and determining the melting point and melting range of the compound by the control system analyzing the change of wrinkles, edges and corners and color space in the image and quantifying the change by using a comprehensive index calculation formula.
Among them, the proposals of patents CN 208060422U, CN 101696948B, CN 205192243U and CN 207007602U can only measure the melting point of colorless and transparent powdery samples; the patents CN 202522530U, CN 203310785U and CN 109444207A can measure the melting point of a colorless and transparent powdery sample and can also measure the melting point of a sample with weak light transmission (namely, light color).
However, the above patents cannot determine the melting point of a color-changeable compound such as arylamine, etc., and the color of a sample rapidly deepens and becomes black with the rise of temperature, so that a light source signal of a full-automatic video melting point instrument cannot penetrate through a sample area in a glass capillary, a detector cannot receive a light signal and cannot indicate an initial melting point and a final melting point, and the melting condition of the sample cannot be observed visually after the color of the sample becomes dark, so that the initial melting point and the final melting point cannot be judged. For example, the p-phenylenediamine sample is white crystals before heating, the color of the sample is rapidly deepened and blackened when the p-phenylenediamine sample is close to the melting point, and a light source signal of a melting point instrument cannot penetrate through a p-phenylenediamine sample area to reach a detector after discoloration, so that the initial melting point and the final melting point of the p-phenylenediamine cannot be accurately detected.
Disclosure of Invention
The invention aims to: the method solves the problem of measuring the melting point of the easily discolored compound, and expands the application range of the full-automatic video melting point instrument.
The invention provides a full-automatic video melting point instrument, which comprises a heating module, a video display, a temperature control module, a glass capillary tube, a light source and a detector, and is characterized in that a metal indicating rod is placed in the glass capillary tube, and the glass capillary tube has the diameter of 0.6-1.5mm and the length of 80-160 mm. The gap between the metal indicating rod and the glass capillary is less than or equal to 0.05mm, the lower part of the metal indicating rod is a cylinder with the length of 5-15mm, the periphery of the bottom of the cylinder is provided with a flow guide opening which is connected with the liquid sample storage area and used for guiding the melted liquid to the sample storage area, the middle part of the metal indicating rod is a cylinder with the height of 100-130mm, the cylinder is provided with a light hole, the distance between the light hole and the liquid sample storage area is 1-10mm, the top end of the metal indicating rod is provided with a 0.1-10g metal balance weight which is connected with the metal indicating rod, a baffle with the adjustable height is arranged between the light source and the sample-loaded glass capillary, and the baffle is provided with an incident light hole.
The working principle of the full-automatic video melting point instrument is that when the temperature of a heating module reaches the melting point of a sample, the sample starts to melt and collapse gradually, a metal indicating rod can extrude the melted liquid sample to a liquid sample storage area under the action of gravity, meanwhile, the lower edge of a light hole in the metal indicating rod is gradually superposed with the upper edge of an incident light hole, part of light penetrates through the superposed area to reach a detector, an initial melting point signal is obtained at the moment, and a final melting point signal is obtained when the light hole is completely superposed with the incident light hole.
The glass capillary sample carrying device of the melting point instrument comprises a glass capillary (figure 1) and a metal indicating rod (figure 2); the gap between the metal indicating rod and the glass capillary is less than or equal to 0.05mm, so that the contact between the sample and air is reduced, and the process that the heated color of the sample is darkened is slowed down. The lower part of the metal indicating rod is a cylinder with the length of 5-15mm, the periphery of the bottom of the cylinder is provided with a flow guide port, the flow guide port is connected with the liquid sample storage area and is used for guiding the melted liquid to the sample storage area, the middle part of the metal indicating rod is a cylinder with the height of 100-130mm, the cylinder is provided with a light transmission hole (figure 4), the distance between the light transmission hole and the liquid sample storage area is 1-10mm, and the light transmission hole is used for enabling an optical signal to pass through and enter the detector. A metal weight of 0.1-10g is connected to the metal indicating rod at the top end of the metal rod, and the metal weight provides a downward pressure to the metal indicating rod, so that the metal indicating rod cannot be lowered due to weak friction between the metal indicating rod and the glass capillary tube and surface tension of the molten liquid. A baffle plate with adjustable height is arranged between a light source and a sample-carrying glass capillary tube, and an incident light hole is formed in the baffle plate, so that the upper edge of the incident light hole is always tangent to the lower edge of the light hole under different sample-carrying quantities, and when the height of the metal indicating rod is lowered, the upper edge of the incident light hole and the lower edge of the light hole are gradually overlapped, more and more light signals are detected by a detector, and the incident light hole and the light hole are completely overlapped until the detected light signals are balanced. When the upper edge of the incident light hole and the lower edge of the light hole are just overlapped, the light signal detected by the detector is regarded as an initial melting point; when the incident light hole and the light transmission hole are completely overlapped, the light signal detected by the detector reaches the balance and is regarded as the final melting point.
A detection method of a full-automatic video melting point instrument comprises the following steps,
(1) placing the glass capillary tube filled with the sample in a melting point instrument, and adjusting the height of a baffle plate to ensure that the upper edge of an incident light hole is exactly tangent to the lower edge of a transmission light hole;
(2) setting a temperature rise program according to the melting point range of the compound, and starting to rise the temperature after the temperature of a melting point instrument is stable;
(3) when the temperature reaches the melting point of the sample, the sample starts to melt and collapse, the lower edge of the light hole gradually coincides with the upper edge of the incident light hole, part of light penetrates through the coinciding area and reaches the detector, namely the initial melting point signal, and when the light hole and the incident light hole completely coincide, the light signal reaching the detector is the final melting point signal.
Compared with the prior art, the method solves the problem of measuring the melting point of the easily discolored compound, avoids errors caused by different sample loading amounts, ensures that the error is less than or equal to 0.3 ℃, simplifies the operation process, ensures the accuracy and precision of the detection result, and simultaneously expands the application range of the full-automatic video melting point instrument.
Drawings
FIG. 1 is a schematic view of the glass capillary structure of a melting point apparatus.
The labels in the figure are: 1 glass capillary, 2 samples.
Fig. 2 is a schematic view of a metal indicator stem.
The labels in the figure are: 3 metal balance weight, 4 metal indicating rods, 5 light holes and 6 liquid sample storage areas.
Fig. 3 is a schematic view of a diversion opening at the bottom of a metal indicating rod.
The labels in the figure are: 7 flow guide openings.
Fig. 4 is a schematic view of an entrance light hole and a light transmission hole.
The labels in the figure are: 5 light holes, 8 light sources, 9 incident light holes, 10 detectors, 11 heating modules and 12 baffles capable of adjusting the height of incident light.
Detailed Description
The technical scheme of the invention is described in detail in the following with reference to the accompanying drawings. This example measures the melting point of p-phenylenediamine.
Fig. 1 is a schematic diagram of a glass capillary of a melting point apparatus, which includes two parts, a glass capillary and a sample. The specification of the glass capillary tube is 0.6mm-1.5mm in diameter and 80-160mm in length.
Fig. 2 is a schematic view of a metal indicating rod, the lower part of which is a cylinder with a length of 5-15mm, and the periphery of the cylinder is provided with a flow guide opening (see fig. 3), and the flow guide opening is connected with a liquid p-phenylenediamine sample storage area and is used for guiding the melted liquid p-phenylenediamine to the sample storage area. A cylinder with the height of 100-130mm is arranged in the middle of the metal indicating rod, a light-transmitting hole is arranged on the cylinder, the distance between the light-transmitting hole and the p-phenylenediamine sample storage area is 1-10mm, and a light source signal penetrates through the light-transmitting hole to reach the detector. When the upper edge of the incident light hole and the lower edge of the light hole are just overlapped, part of light source signals reach the detector through the overlapping area, namely the p-phenylenediamine initial melting point; when the incident light hole and the light hole are completely overlapped, the light signal reaching the detector is the strongest, namely the p-phenylenediamine final melting point. The metal rod is connected with a metal indicating rod by a metal weight of 0.1-10g at the top end of the metal rod, and the metal weight provides downward gravity for the metal rod indicating rod, so that the metal rod cannot descend because of weak friction between the metal rod and a glass capillary tube and the surface tension of liquid p-phenylenediamine after melting.
Fig. 4 is a schematic diagram of an incident light hole and a light transmission hole. A baffle plate with adjustable height is arranged between a light source and a sample-carrying glass capillary tube, and an incident light hole is arranged on the baffle plate, so that the initial upper edge of the incident light hole and the lower edge of a light-transmitting hole can be adjusted to be tangent under different sample-carrying quantities, and the upper edge of the incident light hole and the lower edge of the light-transmitting hole can be gradually coincided when the height of a metal indicating rod is reduced, more and more light signals are detected by a detector, and the incident light hole and the light-transmitting hole are completely coincided until the detected light source signal reaches the maximum value.
The operation steps are as follows:
1. placing the glass capillary tube filled with the p-phenylenediamine sample in the melting point instrument, and adjusting the height of the baffle plate to ensure that the upper edge of the incident light hole is just tangent to the lower edge of the transmission light hole;
2. setting the initial temperature of the melting point instrument to be 138 ℃, the heating rate to be 1.0 ℃/min and the stopping temperature to be 154 ℃;
3. after the temperature of the melting point instrument is stabilized at 138 ℃, the temperature is raised;
4. when a p-phenylenediamine sample starts to melt, liquid p-phenylenediamine is extruded by the metal indicating rod and is guided to the p-phenylenediamine storage area through the guide opening, meanwhile, the metal indicating rod descends, the upper edge of the incident light hole is gradually overlapped with the lower edge of the light hole, the light source signal is detected by the detector, the light source signal is the initial melting point of 146 ℃, the final melting point of 148 ℃ is obtained when the light source signal reaches the maximum value and is stable, the measured melting range of the p-phenylenediamine is 146-148 ℃, and the measured melting range of the p-phenylenediamine is consistent with the theoretical value.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A full-automatic video melting point instrument comprises a heating module, a video display, a temperature control module, a glass capillary tube, a light source and a detector, and is characterized in that a metal indicating rod is placed in the glass capillary tube, the diameter of the glass capillary tube is 0.6-1.5mm, and the length of the glass capillary tube is 80-160 mm; the lower part of the metal indicating rod is a cylinder with the length of 5-15mm, the periphery of the bottom of the cylinder is provided with a flow guide port, the flow guide port is connected with the liquid sample storage area, the middle part of the metal indicating rod is a cylinder with the height of 100-130mm, the cylinder is provided with a light transmission hole, the distance between the light transmission hole and the liquid sample storage area is 1-10mm, the top end of the metal indicating rod is provided with a metal counterweight with the weight of 0.1-10g and connected with the metal indicating rod, a baffle with the adjustable height is arranged between the light source and the sample-carrying glass capillary tube, and the baffle is provided with an incident.
2. The full-automatic video melting point apparatus according to claim 1, wherein the gap between the metal indicating rod and the glass capillary is less than or equal to 0.05 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921360602.2U CN210720215U (en) | 2019-08-21 | 2019-08-21 | Full-automatic video melting point appearance |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921360602.2U CN210720215U (en) | 2019-08-21 | 2019-08-21 | Full-automatic video melting point appearance |
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| CN210720215U true CN210720215U (en) | 2020-06-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110426412A (en) * | 2019-08-21 | 2019-11-08 | 江苏扬农化工集团有限公司 | A kind of full-automatic video melting point apparatus and measuring method |
| CN112304844A (en) * | 2020-10-19 | 2021-02-02 | 西北工业大学 | Method for rapidly measuring initial melting temperature of single crystal high-temperature alloy |
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2019
- 2019-08-21 CN CN201921360602.2U patent/CN210720215U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110426412A (en) * | 2019-08-21 | 2019-11-08 | 江苏扬农化工集团有限公司 | A kind of full-automatic video melting point apparatus and measuring method |
| CN112304844A (en) * | 2020-10-19 | 2021-02-02 | 西北工业大学 | Method for rapidly measuring initial melting temperature of single crystal high-temperature alloy |
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