CN110057855A - Eliminate the device that environmental fluctuating influences simultaneous thermal analysis curve - Google Patents

Eliminate the device that environmental fluctuating influences simultaneous thermal analysis curve Download PDF

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Publication number
CN110057855A
CN110057855A CN201910361276.5A CN201910361276A CN110057855A CN 110057855 A CN110057855 A CN 110057855A CN 201910361276 A CN201910361276 A CN 201910361276A CN 110057855 A CN110057855 A CN 110057855A
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CN
China
Prior art keywords
thermal analysis
analysis curve
simultaneous thermal
furnace body
environmental fluctuating
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CN201910361276.5A
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Chinese (zh)
Inventor
董红娟
刘素霞
高琳
张立
罗龙
刘艳丽
李丽荣
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Inner Mongolia University of Science and Technology
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Inner Mongolia University of Science and Technology
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Priority to CN201910361276.5A priority Critical patent/CN110057855A/en
Publication of CN110057855A publication Critical patent/CN110057855A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means

Abstract

The present invention relates to a kind of devices that elimination environmental fluctuating influences simultaneous thermal analysis curve, and pressure buffer device specially is arranged between synchronous solving and the exhaust outlet of measurement furnace body.The device that elimination environmental fluctuating of the invention influences simultaneous thermal analysis curve, pressure buffer device is set between synchronous solving and the exhaust outlet of measurement furnace body, and the increase of surge flask, so that local resistance substantially increases, kinetic energy increases simultaneously, and pressure energy accounting reduces, and realizes pressure buffer, to realize the Precision measurement under adverse circumstances, the applicability and utilization rate of lifting means.

Description

Eliminate the device that environmental fluctuating influences simultaneous thermal analysis curve
Technical field
The present invention relates to a kind of devices that elimination environmental fluctuating influences simultaneous thermal analysis curve.
Background technique
Synchronous solving STA449C is a instrument of the resistance to production of speeding of Germany.The equipment using platinum rhodium stove heating, The broad temperature range of RT~1650 DEG C can be covered.It is equipped with the ultramicrobalance with electromagnetic compensation, there is high accuracy, g grades of μ Resolution ratio and outstanding stability, and the sample for the 3.5g that weighs can be tested.Temperature control rate is 0.1 DEG C/min~50 DEG C/min, DSC temperature accuracy is ± 0.5 DEG C.Spline structure, vacuum tightness design are filled using top, vacuum degree can reach 10-2Pa.The equipment The shared construction of large-scale instrument and equipment for taking part in Inner Mongolia, assists to complete more areas, multi-disciplinary transverse direction, longitudinal direction, districts and cities Grade and national project.The instrument is wide to cover temperature, and measuring accuracy is high, and feature easy to operate is single in major detection Position, school, research institute are widely applied.
Synchronous solving can get thermogravimetric (TG) and differential thermal (DSC or DTA) information by one-shot measurement.Fig. 1 a is synchronous The structure chart of thermal analyzer.Its experimental principle is: weight and thermal change of the record sample under programed temperature.Fig. 1 b Be the result figure of an oxalic acid hydrate calcium, the sample of 8.035mg put into furnace body, with the heating rate of 10 DEG C/min, from room temperature plus Heat obtains the curve that example weight (TG) and heat (DSC) vary with temperature to 1000 DEG C.According to the size of weight loss in map And the height of reaction temperature, it can clearly judge the decomposable process of an oxalic acid hydrate calcium.
Synchronous solving is used to measure decomposition, absorption, oxidation, reduction, fusing, the solidification, crystallization, core with research material The phase transition process such as change, solidification, glass transition;Specific heat, purity, crystallinity, reaction heat can be calculated;The anti-oxidant of Knowing material lures It leads the phase, kinetics;Identify for substance and ingredient etc..It has been widely used in plastics, rubber, coating, food, doctor The research and development in the fields such as medicine, metallurgy, ceramics, building materials, petroleum, biology, coal chemical industry, cosmetics, glass, macromolecule, technique are excellent Change and quality monitoring.
Heat analysis detection is the important means of material physical property test, and application is especially extensive, is related to every field.Together Step thermal analyzer almost occupies a heat analysis detection cities mostly because being related to wide temperature range, precision height, feature easy to operate ?.
But synchronous solving has some limitations in specifically used.Equipped with the gentle specific heat type DSC in a ten thousandth day The Precision measurement of bracket needs more stable indoor environment, and the dust and sand weather in northern spring tests it environment and proposes challenge. As shown in Figure 1a, synchronous solving needs to be passed through in entire test process protection gas (Protective) and purge gas (Purge1/Purge2).Protective gas is for protecting in operation to heating element, to guarantee that it uses the longevity Life.Purge gass can be used as reaction gas, if sample is decomposed in test process, the circulation of protection gas and purge gass from bottom to top Mode, it is ensured that the timely discharge of decomposition product avoids pollution furnace body and sensor.In order to make to protect gas and reaction gas not shadow The phase transformation reaction of material is rung, gas output pressure is generally 0.03Mpa, and flow velocity is less than 100mL/min, and protection air-flow amount is generally 10mL/min~20mL/min, purge gass flow are generally 20mL/min~30mL/min.However, lesser output pressure and stream Amount is highly susceptible to the influence of indoor environment.The exhaust outlet of equipment is directly connected with room atmosphere, and dust and sand weather easily causes room Interior air pressure is unstable, the fluctuation so that thermal analysis curve is serrated, as shown in Fig. 2, the accuracy of experimental data has been seriously affected, it is right Device systems transformation, reducing environment is particularly important the influence that equipment uses.
Summary of the invention
An object of the present invention is to provide a kind of devices that elimination environmental fluctuating influences simultaneous thermal analysis curve.
The device that a kind of elimination environmental fluctuating of the invention influences simultaneous thermal analysis curve, specially in simultaneous thermal analysis Pressure buffer device is set between instrument and the exhaust outlet for measuring furnace body.
The device that elimination environmental fluctuating of the invention influences simultaneous thermal analysis curve, in synchronous solving and measurement furnace Pressure buffer device is set between the exhaust outlet of body, and the increase of surge flask, so that local resistance substantially increases, while kinetic energy increases Greatly, pressure energy accounting reduces, and pressure buffer is realized, thus the Precision measurement under realizing adverse circumstances, the applicability of lifting means And utilization rate.
In addition, the device that the above-mentioned elimination environmental fluctuating of the present invention influences simultaneous thermal analysis curve, can also have as Under additional technical characteristic:
Further, the pressure buffer device is thin mouth vial, and the volume of the thin mouth vial is 5L~20L.
Further, it is described measurement furnace body exhaust outlet and the thin mouth vial between be connected with diameter be 2.8mm~ The hose of 3.2mm, it is the soft of 1.8mm~2.2mm that diameter is connected between the thin mouth vial and the synchronous solving Pipe.
Further, the volume of the thin mouth vial is 10L, the exhaust outlet and the thin mouth glass of the measurement furnace body The hose that diameter is 3mm is connected between bottle, being connected with diameter between the thin mouth vial and the synchronous solving is The hose of 2mm.
Further, the inlet pressure for measuring furnace body is 0.01MPa~0.1MPa, and flow is 50mL/min~300mL/ min。
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 a is the sectional view of existing synchronous solving;
Fig. 1 b is the simultaneous thermal analysis map of the oxalic acid hydrate calcium obtained using the synchronous solving of Fig. 1 a;
Fig. 2 is the thermal analysis curve of indention fluctuation;
Fig. 3 is the design drawing of surge flask of the invention.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
The invention proposes a kind of devices that elimination environmental fluctuating influences simultaneous thermal analysis curve, are specially synchronizing heat Pressure buffer device is set between analyzer and the exhaust outlet for measuring furnace body.
Advantageously, the pressure buffer device is thin mouth vial, and the volume of the thin mouth vial is 5L~20L.
Advantageously, it is described measurement furnace body exhaust outlet and the thin mouth vial between be connected with diameter be 2.8mm~ The hose of 3.2mm, it is the soft of 1.8mm~2.2mm that diameter is connected between the thin mouth vial and the synchronous solving Pipe.
Advantageously, the volume of the thin mouth vial is 10L, the exhaust outlet and the thin mouth vial of the measurement furnace body Between be connected with diameter be 3mm hose, be connected between the thin mouth vial and the synchronous solving diameter be 2mm Hose.
Advantageously, the inlet pressure for measuring furnace body is 0.01MPa~0.1MPa, and flow is 50mL/min~300mL/ min。
The design of pressure buffer container of the invention uses fluid mechanics knowledge.Hold to effectively analyze pressure buffer The principle of device has intercepted three sections in Fig. 3, has been respectively: air inlet 1, equipment exhaust outlet 2, surge flask gas outlet 3.According to The conservation of energy, three section Bernoulli equation-formula 1 of column.Z is position height, and p is that cross-section pressure, v are that cross-sectional flow, ρ are Density, g are that gravity accelerates, h is on-way resistance and local resistance loss between two sections.
For air, position can z be almost consistent, can ignore, and then develop into each section pressure energy and kinetic energy Transformation-formula 2.
In order to analyze the change in flow of three sections, then continuity equation (the mass-conservation equation)-public affairs of three sections of column Formula 3, A are the area of each section, and v is cross-sectional flow, and assume to be perfect fluid, incompressible.
v1A1=v2A2=v3A3Formula -3
If equipment export does not add surge flask, it is atmospheric pressure that the pressure p of extraneous dusty wind weather, which is constant,;Room air Flow velocity v be also it is constant, be almost equal to zero;By energy equation 2 it is found that outdoor kinetic energy is converted to indoor pressure energy, and then influence The pressure environment of test cabinet causes thermal analysis curve indention to fluctuate.After increasing surge flask, equivalent to increase one Local resistance component;And surge flask discharge area becomes smaller, according to formula 3 it is found that surge flask muzzle velocity increases.Therefore it buffers The increase of bottle, so that local resistance substantially increases, while kinetic energy increases, and pressure energy accounting reduces, and realizes pressure buffer.
The device that elimination environmental fluctuating of the invention influences simultaneous thermal analysis curve, in synchronous solving and measurement furnace Pressure buffer device is set between the exhaust outlet of body, and the increase of surge flask, so that local resistance substantially increases, while kinetic energy increases Greatly, pressure energy accounting reduces, and pressure buffer is realized, thus the Precision measurement under realizing adverse circumstances, the applicability of lifting means And utilization rate.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned Embodiment is changed, modifies, replacement and variant.

Claims (5)

1. a kind of eliminate the device that influences on simultaneous thermal analysis curve of environmental fluctuating, which is characterized in that in synchronous solving and It measures and pressure buffer device is set between the exhaust outlet of furnace body.
2. the device according to claim 1 eliminating environmental fluctuating and being influenced on simultaneous thermal analysis curve, which is characterized in that institute Stating pressure buffer device is thin mouth vial, and the volume of the thin mouth vial is 5L~20L.
3. the device according to claim 2 eliminating environmental fluctuating and being influenced on simultaneous thermal analysis curve, which is characterized in that institute State the hose for being connected with that diameter is 2.8mm~3.2mm between the exhaust outlet and the thin mouth vial of measurement furnace body, the thin mouth The hose that diameter is 1.8mm~2.2mm is connected between vial and the synchronous solving.
4. the device according to claim 3 eliminating environmental fluctuating and being influenced on simultaneous thermal analysis curve, which is characterized in that institute The volume for stating thin mouth vial is 10L, is connected with diameter between the exhaust outlet and the thin mouth vial of the measurement furnace body and is The hose of 3mm is connected with the hose that diameter is 2mm between the thin mouth vial and the synchronous solving.
5. the device according to claim 1 eliminating environmental fluctuating and being influenced on simultaneous thermal analysis curve, which is characterized in that survey The inlet pressure for measuring furnace body is 0.01MPa~0.1MPa, and flow is 50mL/min~300mL/min.
CN201910361276.5A 2019-04-30 2019-04-30 Eliminate the device that environmental fluctuating influences simultaneous thermal analysis curve Pending CN110057855A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5262095A (en) * 1975-11-17 1977-05-23 Seiko Instr & Electronics Ltd Method of slightly decreasing specimen temperature in measurement of h eat quantity, etc.
CN101865868A (en) * 2009-09-28 2010-10-20 中国林业科学研究院木材工业研究所 Differential thermal-gas chromatography combined analysis device
CN108241001A (en) * 2016-12-27 2018-07-03 华润水泥技术研发有限公司 A kind of coal source tracing method
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
US20180284085A1 (en) * 2017-04-03 2018-10-04 Eastman Chemical Company Modified resins and uses thereof
CN109063337A (en) * 2018-08-03 2018-12-21 内蒙古工业大学 A kind of more coupling magnetic field with electric circuit simulation methods of permanent-magnetic wind driven generator

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5262095A (en) * 1975-11-17 1977-05-23 Seiko Instr & Electronics Ltd Method of slightly decreasing specimen temperature in measurement of h eat quantity, etc.
CN101865868A (en) * 2009-09-28 2010-10-20 中国林业科学研究院木材工业研究所 Differential thermal-gas chromatography combined analysis device
CN108241001A (en) * 2016-12-27 2018-07-03 华润水泥技术研发有限公司 A kind of coal source tracing method
US20180284085A1 (en) * 2017-04-03 2018-10-04 Eastman Chemical Company Modified resins and uses thereof
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
CN109063337A (en) * 2018-08-03 2018-12-21 内蒙古工业大学 A kind of more coupling magnetic field with electric circuit simulation methods of permanent-magnetic wind driven generator

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