CN1012845B - Thermal analysing arrangements - Google Patents
Thermal analysing arrangements Download PDFInfo
- Publication number
- CN1012845B CN1012845B CN 86108245 CN86108245A CN1012845B CN 1012845 B CN1012845 B CN 1012845B CN 86108245 CN86108245 CN 86108245 CN 86108245 A CN86108245 A CN 86108245A CN 1012845 B CN1012845 B CN 1012845B
- Authority
- CN
- China
- Prior art keywords
- voltage
- sample
- temp
- specimen
- standard substance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000001514 detection method Methods 0.000 claims abstract description 41
- 239000000126 substance Substances 0.000 claims abstract description 26
- 230000035945 sensitivity Effects 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000002076 thermal analysis method Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000013558 reference substance Substances 0.000 abstract 2
- 230000005669 field effect Effects 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000012546 transfer Methods 0.000 description 6
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
To perform accurate heat analysis by increasing the amplitude of temp. difference voltage of a reference substance and a specimen to correct the lowering component of said amplitude, by multiplying the temp. difference voltage of the reference substance and the specimen by correction voltage. The temp. difference between the standard substance in a standard container showing a characteristic wherein heat quantity detection sensitivity is lowered with the rising in the heating temp. of a heating furnace 1 and the specimen in a specimen container 3 and the temp. of the specimen are separately outputted from thermocouples 5, 5'. Folded line function voltage generators 8-10 output non-linear voltage, wherein a voltage increase rate changes, corresponding to the increase in the specimen temp. voltages outputted from the thermocouples 5, 5' through an amplifier 7 as a correction value. The temp. difference voltage of the standard substance and the specimen from the thermocouples 5, 5' and the correction voltages from the generators 8, 10 are respectively applied to a multiplier 12 through amplifiers 6, 11 and multiplied to correct the lowering in the amplitude of the temp. difference voltage of the standard substance and the specimen.
Description
The invention relates to the apparatus for thermal analysis that has compensation system at output terminal, compensation system compensates the temperature dependency of pick-up unit detection sensitivity.
For example, for the analysis of the state variation of polymer substance, use heat flow flux type differential calorimetric determination device mostly.In this device, the volumetric standard of sampling receptacle that inserts sample and insertion standard substance is placed on the heat transfer plate that places in the heating furnace, make it heating with certain programming rate, the sample heat absorption that takes place in this process and the transmission and the reception of the caused heat energy of heating phenomenon are undertaken by heat transfer plate, meanwhile, the detected differential heat of the pick-up unit that is made of two thermopairs is measured.
In this device, because transmitting and receive the pyroconductivity of the heat transfer plate of heat energy changes with the temperature rising, and heat transmission also is subjected to the influence with factors such as the corresponding radiation of environment temperature, convection current, so the pick-up unit of two thermopair formations shows the characteristic that rises and reduce with heating-up temperature to the heat absorption of sample and the detection sensitivity of heating.Therefore, the amplitude of the peak value waveform of heat absorption of expression sample and heating just reduces with the rising of heating-up temperature.Therefore, although taked in the above and below of heating furnace topped glossiness soaking fragment of brick to prevent the pick-up unit partial heat, but, the heating-up temperature of heating furnace is risen on one side with certain speed since be, measure on one side, just can not be irrelevant with the variation of environment temperature, so the amplitude of output peak value waveform still exists with the problem that temperature changes.
In view of the above problems, the purpose of this invention is to provide a kind of improved apparatus for thermal analysis, its detection sensitivity is compensated, make it not to be subjected to the influence of environment temperature at the output terminal of pick-up unit.
That is to say, feature of the present invention is: be provided with pick-up unit and polygronal function voltage generation circuit, pick-up unit will represent that the heat detection sensitivity exports respectively with the temperature difference and the sample temperature of sample with the heating furnace heating-up temperature standard substance reduce characteristic that rises, the non-linear voltage that polygronal function voltage generation circuit output changes with the increase of the sample temperature voltage of above-mentioned detection device output, meanwhile, also have multiplying device or bleeder mechanism, the multiplying device carries out multiplying to the voltage that above-mentioned polygronal function voltage generation circuit takes place with the standard substance of above-mentioned pick-up unit detection and the thermoelectric voltage of sample, the voltage that bleeder mechanism takes place with above-mentioned polygronal function voltage generation circuit is control voltage, can change with above-mentioned control voltage amplitude by its internal resistance, be transformed to the variable impedance apparatus that has with above-mentioned detection device detection sensitivity characteristic symmetry characteristic, the standard substance of above-mentioned detection device output and the thermoelectric voltage of sample are carried out dividing potential drop.
When the thermoelectric voltage of standard substance that the pick-up unit that the heat detection sensitivity is reduced with the increase of the heating-up temperature of heating furnace detects and sample is defeated by the multiplying device, the non-linear voltage that the rising of the sample temperature voltage that the voltage increment rate is detected with pick-up unit changes is a bucking voltage, also be defeated by the multiplying device, by bucking voltage is carried out multiplying with the thermoelectric voltage of standard substance and sample, to standard substance and sample thermoelectric voltage peak area reduce compensate.
In addition, with above-mentioned non-linear voltage is the control utmost point that control voltage is defeated by variable impedance apparatus, by this control voltage, make the internal resistance acquisition of variable impedance apparatus and the characteristic of pick-up unit detection sensitivity symmetry, thereby output is through the standard substance of the not examined device heat detection sensitivity influence of over-compensation and the thermoelectric voltage of sample.
The 1st figure is the structural drawing of one embodiment of the present of invention, and the 2nd figure (A) is heat detection sensitivity performance diagram and the heat absorption and the peak value oscillogram of generating heat of thermopair, and the 2nd figure (B) is the output voltage waveform of polygronal function voltage generator.
The 3rd figure is the structural drawing of another embodiment of the present invention device, the 4th figure (A) is heat absorption and the heat detection sensitivity family curve of heating and the internal resistance performance diagram behind compensation pmos transistor of thermopair, and the 4th figure (B) is the internal resistance performance diagram crossed without compensation pmos transistor and the output voltage waveform of polygronal function voltage generator.In the drawings:
1 ... heating furnace
5,5 ' ... thermopair
10,8,9 ... the polygronal function voltage generator
12 ... multiplicative operator
15 ... field effect transistor
Below, the embodiment shown in elaborates to the present invention with reference to the accompanying drawings.
What accompanying drawing was represented all is embodiments of the invention, symbol 1 among the 1st figure is a heating furnace, the heat transfer plate made from materials such as copper 2 wherein is housed, inserting the sampling receptacle 3 of sample and the volumetric standard 4 of insertion standard substance is placed on this heat transfer plate 2, simultaneously, also be equipped with on this heat transfer plate 2 thermopair 5 and 5 that is used for test sample temperature and standard substance temperature and the temperature difference of sample temperature and standard substance and sample is exported respectively ', shown in the family curve a of Fig. 2 (A), thermopair 5 and 5 ' the heat detection sensitivity reduce with the rising of heating-up temperature.In addition, in the 2nd figure (A), the standard substance of representing with solid line and the thermoelectric voltage of the sample peak value waveform C in sample heat absorption and heating process, this is received heat detection sensitivity influence and waveform before the compensation that peak area reduces, and what be represented by dotted lines is peak value waveform after over-compensation.6 and 7 is amplifiers, be used for amplifying the sample temperature voltage of the thermopair 5 and 5 ' standard substance of detection and the thermoelectric voltage of sample and thermopair 5 ' detection respectively, amplifier 6 is connected with the X end of multiplicative operator 12, and amplifier 7 joins with polygronal function voltage generator 8～10.The structure of polygronal function voltage generator 8～10 is: resistance R
1～R
3, R
4～R
6And R
7～R
9Three series circuits forming are parallel with one another, simultaneously, are connected to diode D, D respectively at feedback loop and output terminal.Resistance R
2, R
5And R
8An end be connected to operational amplifier OP
1, OP
2And OP
3Input end, their other end links to each other with the output terminal of operational amplifier separately by diode D respectively.Each operational amplifier adopts anti-phase input mode, positive ending grounding, and the bias voltage that size is had nothing in common with each other is added to operational amplifier OP
1～OP
3Inverting input, each bias voltage is taken from the series circuit of being made up of four resistance, the two ends of this series circuit add respectively+15V and-voltage of 15V.Polygronal function voltage generator 8～10 is along with the output voltage of amplifier 7 increases, and at first the resistance loop by above-mentioned each series circuit is together in parallel makes and operational amplifier OP then in proper order
1, OP
2And OP
3The diode D, the D conducting that connect, export the polygronal function voltage curve b that numerical expression is compressed that presses shown in the 2nd figure (B), and be defeated by the Y end of multiplicative operator 12 by amplifier 11, be defeated by not shown data processing equipment through the voltage of multiplying by the Z end.In addition, these voltage generators 8～10 can be exported the non-linear voltage with slope characteristic, and the heat detection sensitivity characteristic that the temperature difference influenced of standard substance and sample is compensated.
In the device that constitutes like this, if the heating-up temperature of heating furnace 1 is risen, the X that the hot temperature voltage of differential of the peak value waveform C after the peak area of thermopair 5 and 5 ' detection of then can be correspondingly the middle solid line of the 2nd figure (A) being represented by amplifier 6 reduces is defeated by multiplicative operator 12 holds.On the other hand, by amplifier 7 the sample temperature voltage of the increase of thermopair 5 detections is defeated by polygronal function voltage generator 8～10.Thus, the output voltage at amplifier 7 reaches V
1Before, electric current just passes through resistance R
1～R
3, R
4～R
6And R
7～R
9The parallel circuit of forming is shunted, and exports the linear voltage shown in the family curve b of the 2nd figure (B), at this voltage from V
1Change to V
2During this time, operational amplifier OP
1Diode D, D conducting, form and resistance R
2Circuit in parallel closes resistance and reduces thereby make, and the output voltage increment rate reduces; Secondly, at voltage from V
2Change to V
3During this time, operational amplifier OP
2Diode D, D conducting, form and resistance R
5Circuit in parallel closes resistance and further reduces, so the output voltage increment rate reduces further; At last, at voltage from V
3Change to V
4During this time, operational amplifier OP
3Diode D, D conducting, form and resistance R
8Circuit in parallel, the output voltage increment rate further reduces.With polygronal function voltage generator 8～10 be bucking voltage to numerical expression compression voltage, be defeated by the Y end of multiplicative operator 12 by amplifier 11.Because the bucking voltage of polygronal function voltage generator 8～10 outputs increases with the rising of sample temperature voltage, so, in multiplicative operator 12, during peak value waveform C that the amplitude of the hot temperature of representing with solid line whenever input of differential reduces, just at this moment bucking voltage value is carried out multiplying as the amplitude of coefficient and this peak value waveform C, the peak value waveform C that thus amplitude is reduced is compensated for as waveform that amplitude that dotted line represents increases then, exports by anode.
Below, another one embodiment of the present invention is described.
The 3rd figure is the device of another one embodiment of the present invention, and it is identical that the part identical with the 1st figure marked symbol.
In the present embodiment, amplifier 6 passes through resistance R
0Be connected with the source electrode of field effect transistor (FET) 15, field effect transistor 15 have the internal resistance shown in the family curve d of the 4th figure (B) with grid voltage 0～Vn by the characteristic that sharply increases linearly, polygronal function voltage generator 8～10 is connected with the grid of field effect transistor 15 by amplifier 11.In addition, the structure of polygronal function voltage generator 8～9 has been considered the detection sensitivity characteristic of detection part and the grid bias and the internal resistance characteristic of field effect transistor 15, thereby, can produce the detection sensitivity and the linear polygronal function voltage of heating-up temperature that make detection part.
The 13rd, amplifier, it the output voltage of amplifier 6 through resistance R
0After field effect transistor 15 dividing potential drops, the dividing potential drop of field effect transistor 15 is defeated by not shown data processing equipment.In addition, the symbol 14 among the figure is the adjustment circuit that add for the characteristic deviation of compensating field effect transistor, is used for adjusting the bias voltage of being defeated by grid.
In the device that constitutes like this,, then correspondingly the thermopair 5 and 5 ' standard substance of detection and the thermoelectric voltage of sample are defeated by the source electrode of field effect transistor 15 by amplifier 6 if the heating-up temperature of heating furnace 1 is risen.On the other hand, by amplifier 7 the sample temperature voltage of the increase of thermopair 5 detections is defeated by polygronal function voltage generator 8～10.Thus, the output voltage at amplifier 7 reaches V
1Before, electric current is just through resistance R
1～R
3, R
4～R
6And R
7～R
9The parallel circuit of forming is shunted, and exports the linear voltage shown in the family curve b of the 2nd figure (B), at this voltage from V
1Change to V
2During this time, operational amplifier OP
1Diode D, D conducting, form and resistance R
2Loop in parallel is closed resistance and is reduced thereby make, so the output voltage increment rate reduces.Thereafter, at voltage from V
2Change to V
3During this time, operational amplifier OP
2Diode D, D conducting, form and resistance R
5Loop in parallel is closed resistance and further reduced, and is last so the output voltage increment rate further reduces, at voltage from V
3Change to V
4During this time, operational amplifier OP
3Diode D, D conducting, form and resistance R
8Loop in parallel, the output voltage increment rate further reduces.Like this because polygronal function voltage generator 8～10th, by amplifier 11 voltage amplitude by numerical expression is compressed into 0～V
4Voltage after be added on the grid of field effect transistor 15, so, shown in the family curve e of the 4th figure (B), compare with the situation of the linear grid voltage 0～Vn of input, its voltage range of field effect transistor is reduced to 0～V
4Simultaneously, internal resistance increment rate in this scope also be subjected to above-mentioned family curve e represented by to the Control of Voltage after the numerical expression compression, so, the detection sensitivity family curve just be compensated for as with the 2nd figure (A) in the 4th figure (A) of a symmetry shown in family curve α '.
Therefore, if field effect transistor 15 is defeated by in the heat absorption of the sample of following amplifier 6 outputs and the peak power of heating, then this peak point current just is defeated by amplifier 13 with the dividing potential drop after multiplying is carried out in the internal resistance of over-compensation, owing to the rising of this dividing potential drop along with heating-up temperature increases, so the peak power that reduces with the rising of heating-up temperature just can be compensated.
In addition, though explanation in the present embodiment is that the detection sensitivity compensation system of detection part is applied to situation in the differential scanning calorimetric determination device, but, this compensation system also can be applied to the differential thermal analysis device, and the quantity of polygronal function voltage generator can suitably increase and decrease according to the requirement of the desirable degree of tilt of broken line voltage.In addition, though the polygronal function voltage generator is to constitute in the mode that the numerical expression compression is reduced according to the voltage increment rate in the present embodiment,,, also can make the form that the voltage increment rate is increased by changing the closure of diode.
As mentioned above, the standard substance that to be bucking voltage export with pick-up unit because the present invention is a non-linear voltage that the voltage increment rate with polygronal function voltage generation circuit output changes and the thermoelectric voltage of sample carry out multiplying, so, even the heat detection sensitivity of pick-up unit reduces with the increase of heating current, and the amplitude that causes the thermoelectric voltage of standard substance and sample thus reduces, also can be by the amplitude of the thermoelectric voltage of standard substance and sample being increased with above-mentioned bucking voltage, thereby compensate the part that it reduces, therefore, can export and be converted into the thermoelectric voltage that not examined unit temp relies on sex standard substance and sample, carry out correct heat analysis.
In addition, owing to be that the sample temperature voltage that pick-up unit detects is defeated by the polygronal function voltage generation circuit, and the voltage increment rate with sample temperature voltage increase reduce by the control utmost point of the non-linear voltage after the numerical expression compression being defeated by variable impedance apparatus for control voltage, so, being added in the control voltage range that the control of variable impedance apparatus extremely goes up has dwindled, can make the characteristic of the detection sensitivity characteristic symmetry of the internal resistance formation of the variable impedance apparatus in this scope and above-mentioned detection device, therefore, can be compensated for as not examined unit temp dependence influence to the peak power of the heat absorption of expression sample and heating, thereby can carry out correct heat analysis.
Claims (1)
1, a kind of apparatus for thermal analysis is characterized in that comprising: pick-up unit, the heat detection sensitivity is exported to a multiplying device respectively with the rise standard substance that reduces and the temperature difference and the sample temperature of sample of the heating-up temperature of heating furnace; The polygronal function device for generating voltage, the non-linear voltage that will change with the increase of the sample temperature voltage of above-mentioned detection device output is also exported to described multiplying device; Multiplying device or bleeder mechanism, described multiplying device carries out multiplying to the voltage that above-mentioned polygronal function device for generating voltage produces with the standard substance of above-mentioned detection device detection and the thermoelectric voltage of sample, the voltage that bleeder mechanism produces with above-mentioned broken line device for generating voltage is control voltage, by variable impedance apparatus the standard substance of above-mentioned detection device output and the thermoelectric voltage of sample are carried out dividing potential drop, the internal resistance of variable impedance apparatus can be transformed to the characteristic that has with the detection sensitivity characteristic symmetry of above-mentioned detection device with the amplitude of above-mentioned control voltage.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29100585A JPH0692947B2 (en) | 1985-12-23 | 1985-12-23 | Thermal analyzer |
| JP291005/85 | 1985-12-23 | ||
| JP60291004A JP2581669B2 (en) | 1985-12-23 | 1985-12-23 | Thermal analyzer |
| JP291004/85 | 1985-12-23 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86108245A CN86108245A (en) | 1987-07-01 |
| CN1012845B true CN1012845B (en) | 1991-06-12 |
Family
ID=26558347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86108245 Expired CN1012845B (en) | 1985-12-23 | 1986-12-22 | Thermal analysing arrangements |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1012845B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009074091A1 (en) * | 2007-12-05 | 2009-06-18 | Chery Automobile Co., Ltd. | A motor torque smoothing treatment method for hybrid power and a hybrid power system |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1494126B1 (en) * | 2003-07-04 | 2007-08-29 | Mettler-Toledo AG | Method and Apparatus for the examination of a material |
| EP2214005B1 (en) | 2009-02-03 | 2019-09-18 | Mettler-Toledo GmbH | Thermo-Analytical Instrument |
-
1986
- 1986-12-22 CN CN 86108245 patent/CN1012845B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009074091A1 (en) * | 2007-12-05 | 2009-06-18 | Chery Automobile Co., Ltd. | A motor torque smoothing treatment method for hybrid power and a hybrid power system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN86108245A (en) | 1987-07-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4058766A (en) | Multiple-frequency permittivity tester | |
| KR101306612B1 (en) | System and method for analyzing power flow in semiconductor plasma generation systems | |
| CN111596184B (en) | Method and device for detecting insulation performance of insulation medium based on electric charge quantity | |
| Liston et al. | A contact modulated amplifier to replace sensitive suspension galvanometers | |
| CN106199366B (en) | A kind of method of power MOS (Metal Oxide Semiconductor) device temperature measurement on-line | |
| CN101738546A (en) | Device, system and method for measuring space charges by using electro-acoustic (PEA) method | |
| US3339398A (en) | High sensitivity differential thermal analysis apparatus and method | |
| US5212453A (en) | Pulse echo method and apparatus for measuring the moisture content of materials | |
| CN1012845B (en) | Thermal analysing arrangements | |
| DE3116244C2 (en) | Process for the aging of SnO 2 semiconductor gas probes and the probes obtained thereby | |
| US5083080A (en) | High frequency signal measuring equipment with cabled detecting and signal companding | |
| US2623106A (en) | Method and apparatus for measuring the time rise and decay time of pulses | |
| CN109655654B (en) | High-current measurement method and device based on bypass shunt technology | |
| US4030840A (en) | Waveform sampler | |
| GB2307559A (en) | Voltage measuring arrangement with an AC/DC converter and calibration means | |
| Merev et al. | Implementation and Analysis of a Reference Partial Discharge Measurement System | |
| US6043465A (en) | Temperature measurement device for furnace heating elements, furnace utilizing said device and method of using the same | |
| Clark | A semiautomatic calorimeter for measurement of effective efficiency of thermistor mounts | |
| US3568057A (en) | Phase measurement apparatus incorporating square wave voltage difference compensation | |
| CN113866579B (en) | Voltage transformer induction withstand voltage test method and device | |
| JP2581669B2 (en) | Thermal analyzer | |
| RU2039956C1 (en) | Device converting physical parameters into electric signal | |
| Verspecht | Broadband sampling oscilloscope characterization with the" nose-to-nose" calibration procedure: a theoretical analysis | |
| US2366628A (en) | Wave frequency monitor | |
| CN86103773A (en) | Microgalvanometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |