SU1515072A1 - Differential microcalorimeter - Google Patents

Abstract

The invention relates to heat engineering and is intended for studies of physicochemical processes. The aim of the invention is to improve the measurement accuracy due to the mutual compensation of heat pulses in the working and reference cells when introducing components and expanding the functionality due to the possibility of studying the physicochemical processes of volatile substances. A loading unit glass with insertable components and a loading unit glass with the equivalent input components are inserted into the respective coils of the windings of electromagnets rigidly fixed in the lids on the side of the reaction containers, and held there by friction force. The lids of the reaction containers are threaded, with which they are screwed onto the reaction containers. The wires connected to the windings of the electromagnets are sealed with a sealant to ensure tightness. The control pulse shaper is a one-shot, which forms a rectangular pulse at the command of the operator. The power supply provides a stabilized voltage to power the driver pulse driver circuit. A rectangular impulse from the driver of the control pulse enters the windings of the electromagnets. At the same time, the rods mechanically connected with the corners of the electromagnets are drawn into the coils, on which the electromagnet windings are located, until the collar coils reach the edges of the coils. The stroke of the rods is chosen so that when the electromagnet koreas move, they push the cups of the loading blocks into the reaction containers. In reaction containers, it is easy to ensure tightness, which allows working with volatile substances. The measurement accuracy is increased by 10 times due to the mutual compensation of heat pulses in the working and reference cells with the introduction of components. 1 il.

Description

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cells with the introduction of components and the expansion of functional capabilities due to the possibility of studying the physicochemical processes of volatile substances. A loading unit glass with the input components and a loading unit glass with the equivalent input components are inserted into the respective coils of the windings of the electromaterials rigidly fixed in the racks on the side of the reaction containers and held there by friction force. The lids of the reaction containers are threaded, with which they are screwed onto the reaction containers. The wires connected to the windings of the electromagnets are sealed with a sealant to ensure tightness. The shaper of the control-; 10H1 (1) H) impulse is one- (11) bib | 1 ;: mountains. forming on the command of the operator 11р м () ugo, 1n impulse. The power supply creates a stabilized;

to power the driver pulse driver circuit. A rectangular impulse from the driver of the control pulse enters the windings of the electromagnets. At the same time, the rods, mechanically connected with the corners of the electromagnets, are drawn into the wires on which the windings of the electromagnets are located, until the beads of the Koreas reach the edges of the coils. The stroke of the rods is chosen so that when the electromagnet koreas move, they push the cups of the loading blocks into the reaction containers. In reaction containers, it is easy to ensure tightness, which allows working with highly volatile substances. The accuracy of measurement increases with 10 times due to the mutual compensation of heat pulses in the working and this one cell with the introduction of components. 1 il.

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The application relates to heat engineering, in particular, to devices of differential microcooses. legal meters, and is intended to D. 1I isg. To donan physical and chemical processes.

lie: ii, improve the accuracy of the measurement due to the mutual compensation of heat pulses in the working and this cell with the introduction of components and the expansion of fucniopalities due to the possibility of investigating the volatile substances.

The drawing shows the differential and m and k) () calimeter.

Di (1nc microcalorimeter contains working 1 and reference 2 cells, reactive ion containers. 5 and 4, blocks 5 and 6 of loading, rods mechanically connected to the cores of electromagnets 7 and 8, windings 9 and 1 (1 vaeKTpoMapHHOBOBj covers 11 and 12 nvoda 13 and 14 reactionary capptyrers placed in ceramic pipes and filled with 1 merik, body 15 of the microscalemeter, which is formed: 1 16 packs of power, 17, sa block 17, power n calorimetric block 18.

Differential. 1 microcalorimeter works as follows.

P) and a differential microcalorimeter workstation, input of components takes place with, 1 ped.): Cup of block 5 with injected components and cup b, about 6 loads with equivalent and | 1x components up, 1С) TC in coils of windings 9 and 10 electromagnets, rigid ( in the lids 11 and 12 from the side of the reaction containers 3 and 4 and holding them; Caps

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11 and 12 reaction containers have 5 threads, with which they are pushed onto reaction containers 3 and 4. Wires 13 and 14, which are connected to windings 9 and 10 of electromagnets, are filled with an airtight seal to ensure tightness.

Reaction containers 3 and 4 with screwed-on lids 11 and 12 are inserted into working 1 and reference 2 cells and thermostats) at a certain temperature, while the amount of heat released or absorbed during physicochemical processes is determined by a measuring circuit with differentially included thermocouple batteries (not shown). The control pulse shaper 16 is a single-pulse oscillator, 0 which forms a rectangular imp on the command of the operator: 1 s, with an amplitude of 10 V and a duration of 10 ms. Power supply 17 creates a stabilized voltage of + 10V to power the driver pulse driver circuit 16. At the operator's command, the windings 9 and 10 of the electromagnets flow directly: a 1 pulse from the driver 16 of the control pulse, while the rods mechanically connected to the corners of the electromagnets 7 and 8 are drawn into the coils on which the windings 9 and 10 of the electromagnets are located until the collar of electromagnet 7 and 8 reaches the edges of catuplek. The stroke of the rods is chosen such that when the koreas of electromagnets 7 and 8 move, they push the cups of the loading blocks into the reaction containers 3 and 4.

In the reaction containers of the differential microcalorimeter.

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Leak-proof, allowing operation with highly volatile substances.

The measurement accuracy is increased by 10 times due to the mutual compensation of heat pulses in the working and reference cells with the introduction of components.

The proposed differential microcalorimeter was used to measure the heats of dissolution of a number of amines in methyl alcohol, while the error was no more than 1%.

When using known differential microcalorimeters (for example, a long rod, going beyond the dimensions of a differential microcalorimeter), the error was no more than 10%.

Claims (1)

Invention Formula A differential microcalorimeter for determining the heat of mixing, containing a thermostatted shell-housing, a calorimetric unit with a working and reference No load cells, load blocks with reaction containers and rods in the working and reference cells, a measuring circuit with differentially connected thermocouple batteries, characterized in that, in order to improve measurement accuracy due to the mutual compensation of heat pulses in the working and reference cells when components are introduced and expansion of functionality due to the provision of research of physicochemical processes of volatile substances, loading blocks are tightly located in the lids of the reaction containers, p placed in the working and reference cells, and made in the form of windings of electromagnets, rigidly fixed in the covers on the axis of which with the possibility of movement in the winding installed measles with a collar without a gap on the side of the cover, and on the side of the reaction container in the winding 0 is placed in the form of separate sections, with the entered components. five