CN110426412A - A kind of full-automatic video melting point apparatus and measuring method - Google Patents
A kind of full-automatic video melting point apparatus and measuring method Download PDFInfo
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- CN110426412A CN110426412A CN201910771795.9A CN201910771795A CN110426412A CN 110426412 A CN110426412 A CN 110426412A CN 201910771795 A CN201910771795 A CN 201910771795A CN 110426412 A CN110426412 A CN 110426412A
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- 238000002844 melting Methods 0.000 title claims abstract description 45
- 230000008018 melting Effects 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 44
- 239000011521 glass Substances 0.000 claims abstract description 34
- 210000001747 pupil Anatomy 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 210000001364 upper extremity Anatomy 0.000 claims description 13
- 230000003287 optical effect Effects 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 7
- 230000008859 change Effects 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 15
- 238000010586 diagram Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000003801 milling Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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Abstract
The present invention provides a kind of full-automatic video melting point apparatus and measuring methods, including, heating module, video display, temperature control modules, capillary glass tube, light source and detector, it is characterized in that, metal indicating arm is placed in capillary glass tube, metal indicating arm lower part is the cylindrical body of long 5-15mm, cylinder bottom surrounding has flow-guiding mouth, flow-guiding mouth is connected with liquid sample storage area, for liquid guide flow after melting to sample storage area, the cylindrical body for being high 100-130mm in the middle part of metal indicating arm, there is a loophole on the cylindrical body, there are metal weights to be connected with metal indicating arm on metal indicating arm top, there is a height-adjustable baffle between light source and the capillary glass tube of load sample, there is an entrance pupil on baffle.The present invention solves the measurement of melting point compound easy to change, avoids different volume containing the sample bring errors, simplifies operating process, guarantees the accuracy and precision of testing result, while also extending the application range of full-automatic video melting point apparatus.
Description
Technical field
The invention belongs to technical field of analytical instruments, and in particular to a kind of device for measuring melting point compound easy to change and survey
Determine method.
Background technique
Fusing point refers to temperature of the crystalline solid when solid-state and liquid are in balance, that is, is transformed from the solidified state into temperature when liquid
Degree.The characteristics such as crystalline solid intermolecular cohesion and lattice energy are to influence the factor of melting point substance.According to structured particles and effect
The difference of power, crystal can be divided into several classes such as molecular crystal, atomic crystal, ionic crystals and metallic crystal, crystalline solid because from
Sub-key, covalent bond, metallic bond and hydrogen bond etc. and combine.When crystalline solid absorbs extraneous energy, chemical bond or intermolecular work
Firmly being destroyed makes crystalline solid become liquid from solid-state.When intermolecular force is weaker or the bond energy of chemical bond is lower, substance
Fusing point it is lower, it is on the contrary then higher.Fusing point is important physical constant, and one of the important method of measurement purity.Therefore, it melts
Point instrument is widely used in chemical industry, medical research.
Widely applied currently on the market is photoelectric detector melting point apparatus, and is continuously available improvement in use.Patent CN
208060422 U devise a kind of dryness storehouse and storehouse of milling, and the magnetron inside dryness storehouse removes wherein raw material microwave heating
Moisture, improve testing precision；The motor of milling for the top of the warehouse of milling drives grinding roller to mill raw material, so that sample particle
It is smaller, more evenly, so that the contact area of hot-air and material in heating process is improved, the time needed for saving test.
101696948 B of patent CN devises a kind of heat-free hysteresis effect capillary melting point apparatus with uniform temperature field, using liquid plus
Thermal medium, electric heating, including heating system and temp measuring system two parts, due to having modified heat stagnation aftereffect by theoretical calculation,
So that fine melt point measurement eliminates thermo-lag systematic error.202522530 U of patent CN uses photoelectric detecting technology, Ji Nengshi
Existing automatic detection function, it may have the function of manually visualizing measurement improves the detection accuracy and reliability of fusing point, expands inspection
Sample range, structure are simple.203310785 U of patent CN devises a kind of video melting point apparatus, which can be intuitively
Displays temperature curve and real-time video image, and the functions such as preservation is realized, plays back, shoot with video-corder, color can be observed by video
Variation and decomposition temperature realize comprehensive integrated INSULATION DESIGN, to make to measure more stable more accurate, it is outer to improve resistance
The ability of boundary's environmental disturbances.205192243 U of patent CN improves melting point apparatus temperature rising module structure, it is by the hair of heating part
Tubule carries out inlaid type installation, when maintenance, only needs to change mold insert, has saved maintenance cost.207007602 U of patent CN
A kind of melting point apparatus capillary sample preparation device is devised, which can guarantee the packed uniform of sample in capillary, so that it is guaranteed that
The accuracy and convenience of experiment, the effective solution sample preparation problem of melting point apparatus capillary, and it is easy for operation.Patent CN
109444207 A describe a set of image recognition software for judging automatically melting point compound, when capturing different by camera
Between under section compound molten state, and the pictorial information captured is fed back into control system and is analyzed, control system is logical
It crosses and the variation of wrinkle, corner angle, color space in image analyze and quantified using overall target calculation formula, thus
Judge the fusing point and melting range of compound.
Wherein 208,060,422 101,696,948 205192243 U and 207007602 U of CN of B, CN of U, CN of patent CN
The scheme of proposition can only measure colorless and transparent powdered samples fusing point；And 202522530 U, CN 203310785 of patent CN
U and 109444207 A of CN can both measure colorless and transparent powdered samples fusing point, can also measure light transmission it is very weak (i.e. color compared with
It is light) fusing point of sample.
But the above patent can not all measure the melting point compound easy to change such as arylamine, because such compound is with the liter of temperature
Height, color sample deepen rapidly blackening, cause the light signal of full-automatic video melting point apparatus can not be through in capillary glass tube
Sample area, detector can not receive optical signal and can not indicate just fusing point and whole fusing point, and color sample deepens afterwards visually
It can not observe sample melted situation, therefore can not also judge just fusing point and whole fusing point.Such as p-phenylenediamine sample is before heating
For white crystal, and when close to fusing point color sample can deepen rapidly, blackening, melting point apparatus light signal can not penetrate after discoloration
P-phenylenediamine sample area reaches detector, so the just fusing point and end fusing point of p-phenylenediamine can not be detected accurately.
Summary of the invention
It is an object of the invention to: it solves the problems, such as melting point compound measurement easy to change, extends full-automatic video melting point apparatus
Application range.
The present invention provides a kind of full-automatic video melting point apparatus, including, heating module, video display, temperature control mould
Block, capillary glass tube, light source and detector, which is characterized in that metal indicating arm, the glass are placed in capillary glass tube
Glass capillary diameter 0.6-1.5mm, long 80-160mm.Gap between the metal indicating arm and capillary glass tube≤
0.05mm, metal indicating arm lower part are the cylindrical body of long 5-15mm, and cylinder bottom surrounding has flow-guiding mouth, flow-guiding mouth and liquid-like
Product storage area is connected, and is high 100-130mm in the middle part of metal indicating arm for liquid guide flow after melting to sample storage area
Cylindrical body, have a loophole on the cylindrical body, loophole is away from liquid sample storage area 1-10mm, on metal indicating arm top
There are the metal weights of a 0.1-10g to be connected with metal indicating arm, have between light source and the capillary glass tube of load sample one it is adjustable
The baffle of height is saved, has an entrance pupil on baffle.
The working principle of full-automatic video melting point apparatus is, when heating block temperature reaches sample fusing point, sample start by
Gradually melt, collapse, metal indicating arm can then squeeze the liquid sample of thawing to liquid sample storage area under the effect of gravity, together
When metal indicating arm on loophole lower edge be gradually overlapped with entrance pupil upper limb, have part light through be overlapped area reach detection
Device is at this time just fusing point signal, is whole fusing point signal when loophole is completely coincident with entrance pupil.
The capillary glass tube load sample device of melting point apparatus includes capillary glass tube (Fig. 1) and metal indicating arm (Fig. 2)；Metal
Gap≤0.05mm between indicating arm and capillary glass tube slows down the heated color of sample and becomes to reduce contact of the sample with air
Deep nigrescence process.Metal indicating arm lower part is the cylindrical body of long 5-15mm, and cylinder bottom surrounding has flow-guiding mouth, flow-guiding mouth and liquid
Aspect product storage area is connected, and is high 100- in the middle part of metal indicating arm for liquid guide flow after melting to sample storage area
The cylindrical body of 130mm has a loophole (Fig. 4) on the cylindrical body, and loophole is away from liquid sample storage area 1-10mm, the light transmission
The effect in hole is optical signal from there through entering detector.There are the metal weights and metal of a 0.1-10g on metallic rod top
Indicating arm be connected, the metal weights to metal indicating arm provide a downward pressure, make metal indicating arm will not because of itself and
Between capillary glass tube after faint frictional force and fusing the surface tension of liquid and can not decline.The glass of light source and load sample
There is a height-adjustable baffle between capillary, there is an entrance pupil on baffle, to guarantee capillary glass tube in difference
Entrance pupil upper limb is tangent with loophole lower edge always under volume containing the sample so that metal indicating arm height decline when, can reach into
It penetrates unthreaded hole upper limb to be overlapped gradually with loophole lower edge, the optical signal that detector detects is more and more, until the optical signal of detection
Entrance pupil is completely coincident with loophole when reaching balance.When entrance pupil upper limb just starts to be overlapped with loophole lower edge, at this time
The optical signal that detector detects is considered as just fusing point；When entrance pupil and loophole are completely coincident, detector is detected at this time
Optical signal reaches balance, is considered as whole fusing point.
A kind of detection method of full-automatic video melting point apparatus, includes the following steps,
(1) capillary glass tube for installing sample is placed in melting point apparatus, and controllable register height, so that entrance pupil upper limb
It is just tangent with transmission unthreaded hole lower edge；
(2) temperature program is set by melting point compound range, is started to warm up after melting point apparatus temperature is stablized；
(3) when temperature reaches sample fusing point, sample starts to melt, collapse, at this time loophole lower edge and entrance pupil upper limb
It is gradually overlapped, there is part light to reach detector, as just fusing point signal through area is overlapped, and when loophole and entrance pupil are complete
The optical signal that detector is reached when coincidence is whole fusing point signal.
Compared with prior art, the present invention solves the measurement of melting point compound easy to change, avoids different volume containing the sample bands
The error come makes its error≤0.3 DEG C, simplifies operating process, guarantees the accuracy and precision of testing result, while also extending
The application range of full-automatic video melting point apparatus.
Detailed description of the invention
Fig. 1 melting point apparatus capillary glass tube structural schematic diagram.
Marked in the figure: 1 capillary glass tube, 2 samples.
Fig. 2 metal indicating arm schematic diagram.
Marked in the figure: 3 metal weights, 4 metal indicating arms, 5 loopholes, 6 liquid sample storage areas.
Fig. 3 metal indicating arm bottom flow-guiding mouth schematic diagram.
Marked in the figure: 7 flow-guiding mouths.
Fig. 4 entrance pupil and loophole schematic diagram.
Marked in the figure: 5 loopholes, 8 light sources, 9 entrance pupils, 10 detectors, 11 heating modules, 12 adjustable incident lights are high
The baffle of degree.
Specific embodiment
With reference to the accompanying drawing, technical solution of the present invention is described in detail.The present embodiment measures the molten of p-phenylenediamine
Point.
As shown in Figure 1 it is the capillary glass tube schematic diagram of melting point apparatus, contains two parts of capillary glass tube and sample.Glass
The specification of glass capillary is diameter 0.6mm-1.5mm, length 80-160mm.
Fig. 2 be metal indicating arm schematic diagram, its underpart be long 5-15mm cylindrical body, cylindrical body surrounding have flow-guiding mouth (see
Fig. 3), flow-guiding mouth is connected with liquid p-phenylenediamine sample storage area, is guided to sample for liquid p-phenylenediamine after melting
Storage area.There is the cylindrical body of an a height of 100-130mm in the middle part of metal indicating arm, has a loophole on the cylindrical body, thoroughly
Unthreaded hole reaches detector through the loophole away from p-phenylenediamine sample storage area 1-10mm, light signal.When entrance pupil upper limb
Just start to be overlapped with loophole lower edge, there is part light signal to reach detector by being overlapped area at this time, as at the beginning of p-phenylenediamine
Fusing point；When entrance pupil and loophole are completely coincident, the optical signal for reaching detector is most strong, as p-phenylenediamine end fusing point.
There are the metal weights of a 0.1-10g to be connected with metal indicating arm on metallic rod top, the metal weights are to metallic rod indicating arm
One downward gravity is provided, makes metal indicating arm will not be because of its frictional force and fusing faint between capillary glass tube
Afterwards the surface tension of liquid p-phenylenediamine and can not decline.
If Fig. 4 is entrance pupil and loophole schematic diagram.There is one to be adjusted between light source and the capillary glass tube of load sample
The baffle of height has an entrance pupil on baffle, to guarantee capillary glass tube entrance pupil beginning upper limb under different volumes containing the sample
Eventually be adjustable to loophole lower edge it is tangent, with guarantee metal indicating arm height decline when, can guarantee entrance pupil upper limb
It is gradually overlapped with loophole lower edge, the optical signal that detector detects is more and more, until the light signal of detection reaches maximum
Entrance pupil is completely coincident with loophole when value.
Operating procedure is as follows:
1. the capillary glass tube for installing p-phenylenediamine sample is placed in above-mentioned melting point apparatus, and controllable register height, so that
Entrance pupil upper limb and transmission unthreaded hole lower edge are just tangent；
2. setting above-mentioned melting point apparatus initial temperature as 138 DEG C, heating rate is 1.0 DEG C/min, and stopping temperature is 154 DEG C；
3. being started to warm up after melting point apparatus temperature is stablized at 138 DEG C；
4. liquid p-phenylenediamine is squeezed by metal indicating arm, is drained by flow-guiding mouth when p-phenylenediamine sample starts fusing
To p-phenylenediamine storage area, while metal indicating arm declines therewith, and entrance pupil upper limb is gradually overlapped with loophole lower edge, at this time
Detector detects light signal, this is 146 DEG C of just fusing point, is whole fusing point after light signal reaches maximum value and stablizes
148 DEG C, actual measurement p-phenylenediamine melting range is 146~148 DEG C, consistent with theoretical value.
The foregoing is merely presently preferred embodiments of the present invention, all in spirit and original of the invention not to limit the present invention
Within then, any modification, equivalent replacement, improvement and so on be should be included within the scope of the present invention.
Claims (3)
1. a kind of full-automatic video melting point apparatus, including heating module, video display, temperature control modules, capillary glass tube, light
Source and detector, which is characterized in that metal indicating arm, the capillary glass tube diameter 0.6- are placed in capillary glass tube
1.5mm, long 80-160mm；Metal indicating arm lower part is the cylindrical body of long 5-15mm, and cylinder bottom surrounding has flow-guiding mouth, water conservancy diversion
Mouth is connected with liquid sample storage area, is the cylindrical body of high 100-130mm in the middle part of metal indicating arm, has one on the cylindrical body
A loophole, loophole have the metal weights of a 0.1-10g away from liquid sample storage area 1-10mm, on metal indicating arm top
It is connected with metal indicating arm, has a height-adjustable baffle between light source and the capillary glass tube of load sample, have one on baffle
A entrance pupil.
2. a kind of full-automatic video melting point apparatus according to claim 1, which is characterized in that the metal indicating arm and glass
Gap≤0.05mm between glass capillary.
3. a kind of detection method of full-automatic video melting point apparatus, including the following steps:
(1) capillary glass tube for installing sample is placed in melting point apparatus, and controllable register height so that entrance pupil upper limb and thoroughly
It is just tangent to penetrate unthreaded hole lower edge；
(2) temperature program is set by melting point compound range, is started to warm up after melting point apparatus temperature is stablized；
(3) when temperature reaches sample fusing point, sample starts to melt, collapse, and loophole lower edge and entrance pupil upper limb be gradually at this time
It is overlapped, there is part light to reach detector, as just fusing point signal through area is overlapped, when loophole is completely coincident with entrance pupil
The optical signal for reaching detector is whole fusing point signal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111398333A (en) * | 2020-04-13 | 2020-07-10 | 中国科学院金属研究所 | Differential thermal analysis method for measuring primary melting temperature of single crystal superalloy |
| 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 CN201910771795.9A patent/CN110426412A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111398333A (en) * | 2020-04-13 | 2020-07-10 | 中国科学院金属研究所 | Differential thermal analysis method for measuring primary melting temperature of single crystal superalloy |
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| 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 |
| CN112304844B (en) * | 2020-10-19 | 2021-07-02 | 西北工业大学 | Method for rapidly measuring initial melting temperature of single crystal high-temperature alloy |
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