CN102759545A - Single group-component differential scanning calorimeter - Google Patents
Single group-component differential scanning calorimeter Download PDFInfo
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- CN102759545A CN102759545A CN2012102548882A CN201210254888A CN102759545A CN 102759545 A CN102759545 A CN 102759545A CN 2012102548882 A CN2012102548882 A CN 2012102548882A CN 201210254888 A CN201210254888 A CN 201210254888A CN 102759545 A CN102759545 A CN 102759545A
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Abstract
The invention belongs to the technical field of thermoanalysis, and discloses a single group-component differential scanning calorimeter, which adopts the single group-component design, and removes a reference unit in the traditional differential scanning calorimeter. The sample unit of the instrument includes an inner crucible and an outer crucible; and the inner and the outer crucibles are made of materials with ultrahigh heat conduction coefficients to guarantee that the two crucibles are provided with uniformly distributed temperature fields during the heating and cooling. Heat flow flowing in or out of a sample can be calculated through the measured temperature between the inner and the outer crucibles, during the measurement, the heat flow is definitely defined, and a big thermal-resistance heat flow passage between the inner and the outer crucibles improves the signal-to-noise ratio of the measurement, so as to improve the accuracy and recurrence rate of the measurement; and the single group-component differential scanning calorimetry is not only suitable for differential scanning calorimeters (DSC), but also suitable for differential thermal analyzers (DTA), thermogravimetry-differential scanning calorimeters (TG-DSC) and thermogravimetry-differential thermal analyzers (TG-DSC).
Description
Technical field
The invention belongs to the thermoanalysis technology field, relate to a kind of thermal analyzer of measuring the sample thermophysical property along with temperature variation, particularly a kind of single constituent element differential scanning calorimeter.
Background technology
Differential scanning calorimetric technology (Differential Scanning Calorimetry; DSC) be meant: under controlled heating and cooling environment; Measure input (output) to measured matter and the energy of reference substance and the relation of temperature, come to confirm the hot physics and the chemical property of material to be detected according to this.
But utilize the hot physics of this technology quantitative measurment material, chemical property, as: thermal capacitance, phase transition temperature, crystallization latent heat etc.
Since 1960's, at first to have released by U.S. Perkin-Elmer since the DSC-1 of the said firm, many instrument companies priorities such as (like Du Ponts) has been released the DSC of multiple model to market.Although the DSC that each company releases is various,, can be divided into two big models: hot flow type and energy compensating formula with regard to its ultimate principle.
Hot flow type differential scanning calorimetric instrument is below sample unit and reference unit, to establish a heat flux plates, and when well heater heated under programmed control, heat was delivered to sample and object of reference through heat flux plates.Through measuring hot-fluid and the sample temperature that flows into testee and object of reference, pass through suitable conversion again.The hot physicochemical property of sample just can be expressed.The major advantage of this method is that the shape to sample does not require.
Energy compensating formula differential scanning calorimeter specific heat streaming DSC is many, and two little well heaters are close to respectively below the sample reference substance thermal resistance, the power through regulating these two little well heaters with compensation sample and object of reference owing to the caused temperature difference of different rerum naturas.
Existing commercial apparatus existing problems and weak point:
There is following weak point in the double plate design (sample unit and reference unit) of hot flow type differential scanning calorimeter and energy compensating formula differential scanning calorimeter:
(1). because the thermal interaction of sample unit and reference unit, the hot-fluid that causes measuring can not reflect really that the rerum natura of sample changes, but by a kind of information of being blured (smeared).
(2) the measurement temperature of instrument can not really be reacted the true temperature of testee.
Summary of the invention
The objective of the invention is to existing hot flow type differential scanning calorimeter and energy compensating formula differential scanning calorimeter weak point, and a kind of single constituent element differential scanning calorimeter of having removed the reference unit in the traditional differential scanning calorimeter that proposes.
The technical matters that the present invention will solve is: adopt single constituent element design, removed the reference unit in the traditional differential scanning calorimeter.
Main technical schemes of the present invention: single constituent element differential scanning calorimeter, its characteristics are that this instrument adopts single constituent element design, have removed the reference unit in the traditional differential scanning calorimeter; The sample unit of instrument comprises inside and outside two crucibles; Inside and outside two crucibles have equally distributed temperature field by the material preparation of super-high heat-conductive coefficient to guarantee two crucibles in the heating and cooling process.
Usually, the sample unit of instrument according to the invention is by interior, and outer two crucibles are formed; The internal diameter of outer crucible is 10-20mm; External diameter is 14-24mm, highly is 10-30mm, and disc plate that up and down a thickness to be arranged respectively be 1-4mm and outer crucible form the isothermal body of a sealing; The internal diameter of interior crucible is 4-10mm, and external diameter is 6-14mm, highly is 5-15mm, and disc plate that up and down a thickness to be arranged respectively be 1-4mm and interior crucible form the isothermal body of a sealing.
Usually, sample is displayed in interior crucible during measurement.1-6 thermopair is inserted into the temperature that outer crucible 1/3 – 2/3 highly measured and controlled outer crucible; The temperature of crucible in crucible 1/3 – 2/3 highly measured and controls in 1-6 thermopair was inserted into, 1 sample thermopair is inserted into the temperature of sample 0-2/3 height measuring samples.
Instrument of the present invention through measure between interior, the temperature of outer crucible is calculated the hot-fluid that flows into or flow out sample.In measurement, hot-fluid is through what clearly define, and between interior, the big thermal resistance heat passage between the outer crucible improves the signal to noise ratio (S/N ratio) of measurement, thereby improves accuracy and the recall factor of measuring.
Single constituent element differential scanning calorimetric technology of the present invention is not only applicable to differential scanning calorimetric instrument (DSC), and is applicable to differential thermal analysis (DTA) instrument (DTA), thermogravimetric-differential scanning calorimetric instrument (TG-DSC), thermogravimetric-differential thermal analysis (DTA) instrument (TG-DSC).
The present invention does not address part and is applicable to prior art.
Description of drawings
Accompanying drawing 1 is the structural representation of the single constituent element differential scanning of embodiment of the invention calorimeter; Accompanying drawing 2 is the fine aluminium fusing of employing embodiment of the invention measurement and the heat content and the thermal capacitance curve map of process of setting; The hot-fluid that accompanying drawing 3 is measured for existing double plate designs an apparatus and the curve map of temperature.
In the accompanying drawing, the 1-outer crucible; The 2-sample; Crucible in the 3-; The 4-thermopair.
Embodiment
Provide practical implementation case of the present invention below, with nearly step narration the present invention, but it does not limit claim of the present invention.
Case study on implementation 1:
Present embodiment is shown in accompanying drawing 1; Crucible 3, outer crucible 1 in the sample unit of single constituent element differential scanning calorimeter mainly comprises, interior crucible 3 and outer crucible 1 have equally distributed temperature field by the material preparation of super-high heat-conductive coefficient to guarantee two crucibles in the heating and cooling process.
The internal diameter of outer crucible 1 is 10mm, and external diameter is 14mm, highly is 14mm, and disc plate that up and down a thickness to be arranged respectively be 1mm and outer crucible 1 form the isothermal body of a sealing; The internal diameter of interior crucible 3 is 4mm, and external diameter is 6mm, highly is the isothermal body of the 6mm disc plate that up and down a thickness to be arranged respectively be 1mm with a sealing of interior crucible 3 formation; Sample 2 is displayed in interior crucible 3.1 thermopair 4 is inserted into the temperature that outer crucible 1 was highly measured and controlled to outer crucible 1/3; The temperature of crucible 3 in crucible 1/3 was highly measured and controlled in 1 thermopair 4 was inserted into, 1 sample thermopair 4 is inserted into the temperature of sample 1/3 height measuring samples 2.
Case study on implementation 2:
The internal diameter of present embodiment outer crucible 1 is 18mm, and external diameter is 22mm, highly is 20mm, and disc plate that up and down a thickness to be arranged respectively be 2mm and outer crucible 1 form the isothermal body of a sealing; The internal diameter of interior crucible 3 is 10mm, and external diameter is 14mm, highly is the isothermal body of the 10mm disc plate that up and down a thickness to be arranged respectively be 2mm with a sealing of interior crucible 3 formation; Sample 2 is displayed in interior crucible 3.6 thermopairs 4 are inserted into the temperature that outer crucible 1 was highly measured and controlled to outer crucible 1/3; The temperature of crucible 3 in crucible 1/3 was highly measured and controlled in 6 thermopairs 4 were inserted into, 1 sample thermopair 4 is inserted into the temperature of sample 1/2 height measuring samples 2.
The application implementation example:
Adopt fine aluminium (99.9999wt%) fusing of embodiment of the invention apparatus measures and the heat content and the thermal capacitance of process of setting to see Fig. 2, as a comparison, adopt the experimental result of double plate design to see Fig. 3.Contrast and experiment can find that the present invention can eliminate the phenomenon that the normal measurement result that occurs is blured (smeard) in double plate designs an apparatus automatically. because instrument of the present invention is measured hot-fluid under the condition of maximum thermal resistance, improved the degree of accuracy of measuring.The measurement crystallization latent heat of instrument of the present invention and the accuracy rate of thermal capacitance are respectively 1% and 3%.The instrument recall factor is higher than 99%.See table 1.
Table 1 fine aluminium measurement data of the present invention
List of references. 1.Hultgren?R,?Desai?P?D?and?Hawkins?D?T,?1973,?
Selected?Values?of?the?Thermodynamic?Properties?of?Elements.?ASM,?Ohio。
Claims (4)
1. a single constituent element differential scanning calorimeter is characterized in that this instrument adopts single constituent element design, has removed the reference unit in the traditional differential scanning calorimeter; The sample unit of instrument comprises inside and outside two crucibles; Inside and outside two crucibles have equally distributed temperature field by the material preparation of super-high heat-conductive coefficient to guarantee two crucibles in the heating and cooling process.
2. single constituent element differential scanning calorimeter as claimed in claim 1; The internal diameter that it is characterized in that said outer crucible is 10-20mm; External diameter is 14-24mm, highly is 10-30mm, and disc plate that up and down a thickness to be arranged respectively be 1-4mm and outer crucible form the isothermal body of a sealing; The internal diameter of crucible is 4-10mm in said, and external diameter is 6-14mm, highly is 5-15mm, the disc plate that up and down a thickness to be arranged respectively be 1-4mm and the isothermal body of a sealing of interior crucible formation.
3. single constituent element differential scanning calorimeter as claimed in claim 1 is characterized in that calculating the hot-fluid that flows into or flow out sample through measuring and control the temperature of two crucibles; In measurement, hot-fluid improves the signal to noise ratio (S/N ratio) of measurement through the big thermal resistance heat passage that clearly defines.
4. according to claim 2 or 3 described single constituent element differential scanning calorimeters; It is characterized in that sample displays in interior crucible; 1-6 thermopair is inserted into the temperature that outer crucible 1/3 – 2/3 highly measured and controlled outer crucible; The temperature of crucible in crucible 1/3 – 2/3 highly measured and controls in 1-6 thermopair was inserted into, 1 sample thermopair is inserted into the temperature of sample 0-2/3 height measuring samples.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568796A (en) * | 2015-10-08 | 2017-04-19 | 耐驰-仪器制造有限公司 | MEMS Bio-DSC |
| US10466189B2 (en) | 2017-04-21 | 2019-11-05 | Board Of Trustees Of Northern Illinois University | Uniform chilling calorimeter system |
| CN112557234A (en) * | 2019-09-25 | 2021-03-26 | 耐驰-仪器制造有限公司 | Thermal analysis apparatus, sample holder assembly and thermal analysis method |
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| DE3221548A1 (en) * | 1982-06-08 | 1983-12-08 | Milan Dr.rer.nat. 7808 Waldkirch Smisek | Combustion calorimeter |
| WO2007017897A2 (en) * | 2005-05-25 | 2007-02-15 | Ipca Laboratories Ltd. | Novel crystalline forms of (s)-n-(1-carboxy-2-methyl-prop-1-yl)-n-pentanoyl-n-[2'-(1h-tetrazol-5-yl)bi-phenyl-4-ylmethyl]-amine |
| CN101063665A (en) * | 2007-05-31 | 2007-10-31 | 湖南三德科技发展有限公司 | Method for measuring heat productivity of heating substance for calorimeter |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
| CN202133634U (en) * | 2011-04-14 | 2012-02-01 | 中山大学 | Testing device for testing roof insulation modules and material properties |
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2012
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Patent Citations (5)
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| DE3221548A1 (en) * | 1982-06-08 | 1983-12-08 | Milan Dr.rer.nat. 7808 Waldkirch Smisek | Combustion calorimeter |
| WO2007017897A2 (en) * | 2005-05-25 | 2007-02-15 | Ipca Laboratories Ltd. | Novel crystalline forms of (s)-n-(1-carboxy-2-methyl-prop-1-yl)-n-pentanoyl-n-[2'-(1h-tetrazol-5-yl)bi-phenyl-4-ylmethyl]-amine |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
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| CN202133634U (en) * | 2011-04-14 | 2012-02-01 | 中山大学 | Testing device for testing roof insulation modules and material properties |
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| 长沙三德实业有限公司等: "带螺旋管的各点等温SDC311/5015量热仪", 《湖北省电机工程学会电厂化学专委会2007年学术年会论文集》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568796A (en) * | 2015-10-08 | 2017-04-19 | 耐驰-仪器制造有限公司 | MEMS Bio-DSC |
| US10466189B2 (en) | 2017-04-21 | 2019-11-05 | Board Of Trustees Of Northern Illinois University | Uniform chilling calorimeter system |
| CN112557234A (en) * | 2019-09-25 | 2021-03-26 | 耐驰-仪器制造有限公司 | Thermal analysis apparatus, sample holder assembly and thermal analysis method |
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