CN209132078U - Apparatus for heating thermoplastic samples - Google Patents

Abstract

The utility model provides a kind of device of heating thermoplastic plastic sample, including shell, upper cover plate, bottom end chamber, top cavity, snap component, capillary, microcapillary tube adapter, interface flange, heated beam, sealing ring, heat-insulating shield.Bottom end chamber is connected by sealing ring with snap component lock sealing with top cavity, and bottom end chamber is mounted on the shell of shell and upper cover plate composition；Capillary is connect by capillary adapter and interface flange with top cavity；Heated beam is fixedly mounted on the intracavitary portion in bottom end by heat-insulating shield；Heated beam is further fitted with crucible, heating rod and temperature sensor, is respectively used to the holding of sample, heats and thermometric；Temperature controller device, solid-state relay are further fitted on shell, for control and displays temperature.At a set temperature, pyrolysis devolatilization simultaneously introduces spectrometer analysis by capillary to thermoplastic sample.The utility model is structurally reasonable simple, and maintenance is easy to make, and heating space sealing avoids the cross contamination and loss of sample.

Description

Apparatus for heating thermoplastic samples

technical field

The utility model relates to a pretreatment device for mass spectrometry analysis, in particular to a device for heating thermoplastic samples, in particular to a device for rapidly heating thermoplastic samples.

Background technique

When thermoplastics are heated or burned, they will pyrolyze to produce odorous fumes, which contain toxic and harmful substances. Thermoplastics at different temperatures have many changes and differences in the toxic components released by their pyrolysis. Study the types and concentrations of toxic components released by thermoplastics under different temperature processing conditions, and provide air quality evaluation for such processing sites. The basis has a certain meaning.

At present, due to the limitations of detection methods and on-site sampling conditions, the detection indicators of toxic components of thermoplastics in processing sites at home and abroad are very limited.

In gas detection technology, mass spectrometry detection technology can provide rich material structure information, with high resolution and qualitative capabilities, while miniaturized mass spectrometers combined with ion bombardment ionization sources and ion trap mass analyzers are widely used in job sites. The method of capillary injection to detect gaseous substances cannot meet the direct injection analysis of thermoplastics.

Utility model content

In view of the defects in the prior art, the purpose of the present invention is to provide a device for heating thermoplastic samples.

A device for heating thermoplastic plastic samples provided according to the utility model comprises a casing, an upper cover plate, a bottom end cavity, an upper top cavity, and a heating column;

The shell and the upper cover are connected to form a hollow cavity;

The bottom end cavity is set above the upper cover plate, the upper top cavity is set above the bottom end cavity, and the bottom end cavity and the upper top cavity are detachably connected or movably connected; The air port is connected to the outside;

The heating column is arranged in the cavity formed by the bottom cavity and the upper top cavity, and the heating column is provided with a sample accommodating groove; the heating column is fastened to the bottom cavity, and the notch of the sample accommodating groove and the exhaust port There are gaps in between.

Preferably, a heating rod is included; the heating rod is arranged on a heating column.

Preferably, the bottom end cavity and the upper top cavity are connected by a snap assembly.

Preferably, it includes a crucible, one end of the heating column is provided with a groove matching the crucible, and the other end of the heating column is provided with a mounting hole matching the heating rod and a mounting hole matching the temperature sensor.

Preferably, it includes a first sealing ring, a second sealing ring, and an interface flange;

The interface flange is installed on the top cover of the top chamber;

The upper top cavity is sealedly connected with the bottom cavity through the first sealing ring;

The upper top cavity is sealedly connected with the interface flange through the second sealing ring.

Preferably, it includes an inner insulation board and an outer insulation board;

The heating column is installed in the bottom end cavity through the inner heat insulating plate;

The shell is installed at the bottom of the bottom end cavity through the outer insulation board;

Preferably, a connecting pipe is included;

The connecting pipe is airtightly connected with the interface flange, and the connecting pipe is communicated with the exhaust port; the connecting pipe is a capillary.

Preferably, a pipe adapter is included; one end of the pipe adapter is connected to the exhaust port through the interface flange, and the other end is connected to the connecting pipe.

Preferably, the chambers of the bottom end chamber and the chambers of the upper top chamber are isolated from each other.

Preferably, it includes relays, electrical connectors, temperature control instruments, temperature sensors, and heating rods;

The heating column is connected with the heating rod, and the heating column is connected with the temperature sensor;

The temperature control instrument is connected to the temperature sensor through the electrical connector; the relay output end of the temperature control instrument is connected to the control signal input end of the relay; in the output circuit of the controlled system of the relay, one pole of the load output end of the relay is connected to the positive pole of the power supply, and the other pole is connected to the positive pole of the power supply. The pole is connected to one end of the heating rod through the electric connector, and the other end of the heating rod is connected to the negative pole of the power supply through the electric connector;

The relay is arranged in the hollow cavity formed by the connection between the shell and the upper cover;

The temperature control instrument is arranged on the front panel of the housing, and the electrical connector is arranged at the bottom of the bottom end cavity.

Compared with the prior art, the utility model has the following beneficial effects:

1. The structure is reasonable and simple, and the maintenance and production are convenient.

2. The crucible is easy to replace, and different crucibles can be replaced according to different samples to avoid cross-contamination of the samples; the crucibles make the samples pyrolyzed and gasified for direct injection and analysis of the miniaturized mass spectrometer.

3. The heating space is sealed, so that volatile organic compounds cannot diffuse outward, which not only avoids the loss of analysis samples, but also ensures that operators will not suck harmful gas components.

4. Meet the sampling requirements of miniaturized mass spectrometers.

The further improvement based on the utility model also helps to realize the integration of temperature display and control, more accurate and effective control of the heating temperature of different thermoplastic samples, and good repeatability of the experiment.

Description of drawings

Other features, objects and advantages of the present invention will become more apparent by reading the detailed description of non-limiting embodiments with reference to the following drawings:

Fig. 1 is the schematic diagram of the device for heating thermoplastic plastic samples provided by the utility model;

FIG. 2 is a partial cross-sectional view of the device for heating a thermoplastic plastic sample provided by the present invention.

The figure shows:

Detailed ways

The present utility model will be described in detail below with reference to specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. It should be noted that, for those skilled in the art, several changes and improvements can be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.

Thermoplastics refer to plastics that melt after heating, form after cooling, and melt again when heated, that is, they have the characteristics of softening by heating and hardening by cooling. It is often heated or even burned in places involving plastic processing such as shoe factories, toy factories, cable factories, etc., and the workshop temperature of the processing place is high. It will be gradually pyrolyzed to produce odorous fumes, most of which are toxic and harmful substances. Thermoplastics have many changes and differences in the toxic components released by their pyrolysis at different temperatures.

Mass spectrometry detection identifies the types of substances through vaporization ionization, separation, and detection of ions of the sample, provides rich material structure information, and has high resolution and qualitative capabilities. Miniaturized mass spectrometers use capillary injection as the direct injection method of the ionization source of the mass spectrometer. As shown in FIG. 1 and FIG. 2 , the utility model provides a device for heating a thermoplastic sample, which enables the thermoplastic sample to be pyrolyzed and gasified through a closed space for direct sample injection and analysis by a miniaturized mass spectrometer.

As shown in FIG. 1 and FIG. 2 , a device for heating thermoplastic plastic samples provided by the present invention includes a casing 1, an upper cover plate 2, a bottom end cavity 3, an upper top cavity 4, a heating column 19, and a heating rod 16; The shell 1 and the upper cover plate 2 together form a hollow cavity, the bottom end cavity 3 is arranged above the upper cover plate 2, the upper top cavity 4 is arranged above the bottom end cavity 3, and the bottom end cavity 3 and the upper top cavity 4 are detachably connected Or flexibly connected; the upper top cavity 4 has an exhaust port 22, and the chamber of the upper top cavity 4 is connected to the outside through the exhaust port 22; the heating column 19 is placed in the cavity formed by the bottom end cavity 3 and the upper top cavity 4, heating The column 19 is provided with a sample accommodating groove; the heating column 19 is fastened to the bottom cavity 3, and there is a gap between the notch of the sample accommodating groove and the exhaust port 22, which is used for degassing the thermoplastic sample Afterwards, the converted gas can be passed to the exhaust port 22 for direct injection and analysis of the miniaturized mass spectrometer. Preferably, the crucible 18 is placed in the sample accommodating groove provided on the heating column 19 for containing the sample, and the cross-contamination and loss of the sample can be avoided. Specifically, as shown in FIG. 1 and FIG. 2 , the bottom cavity 3 and the upper top cavity 4 are connected by a snap assembly 5 . Preferably, the snap-fit assembly 5 may adopt other detachable connection or active connection methods, so that the bottom end cavity 3 and the upper top cavity 4 can be tightly connected.

Specifically, as shown in FIG. 2 , the device for heating a thermoplastic sample includes a crucible 18 , one end of the heating column 19 is provided with a groove matching the crucible 18 , and the other end of the heating column 19 is provided with a matching groove with the heating rod 16 . Mounting holes and mounting holes matching the temperature sensor 20; preferably, one end of the heating column 19 has a groove matching the crucible 18, and the other end has three mounting holes for the heating rods 16 and one mounting hole for the temperature sensor 20; preferably , the temperature sensor 20 is PT100; preferably, the material of the crucible 18 is 304 stainless steel.

The device for heating the thermoplastic sample includes a first sealing ring 15, a second sealing ring 17, and an interface flange 8; the interface flange 8 is installed on the upper cover of the upper top chamber 4; the first sealing ring 15 is installed on the upper top chamber 4 At the connection gap with the bottom end cavity 3, the upper top cavity 4 is tightly connected with the bottom end cavity 3; the second sealing ring 17 is installed at the connection gap between the upper top cavity 4 and the interface flange 8, so that the upper top cavity 4 and the bottom end cavity 3 are tightly connected; The interface flange 8 is tightly connected.

The device for heating the thermoplastic sample includes an inner insulation plate 14 and an outer insulation plate 13; the heating column 19 is installed in the bottom end cavity 3 through the inner insulation plate 14; Insulation; the shell 1 is installed at the bottom of the bottom end cavity 3 through the outer heat insulation plate 13; the outer heat insulation plate 13 is installed at the bottom of the bottom end cavity 3 for thermal insulation between the bottom end cavity 3 and the shell 1; preferably, it includes a support plate 12, The support plate 12 is installed on the casing 1 for fixing and supporting the outer heat insulating plate 13 .

The device for heating a thermoplastic sample includes a connecting pipe 6; the connecting pipe 6 is tightly connected with the interface flange 8, and the connecting pipe 6 communicates with the exhaust port 22; preferably, the connecting pipe 6 is a capillary. The device for heating the thermoplastic sample includes a pipe adapter 7; one end of the pipe adapter 7 is connected to the exhaust port 22 through the interface flange 8, and the other end is connected to a connecting pipe 6; preferably, the connecting pipe 6 is a capillary. Preferably, auxiliary heating wires are added outside the capillary to improve the transmission efficiency of gaseous substances in the capillary. For the device for heating the thermoplastic sample, the chamber of the bottom end chamber 3 and the chamber of the upper top chamber 4 are isolated from each other; preferably, the device for heating the thermoplastic sample includes a support pad 21 .

In a preferred example, the device for heating a thermoplastic sample includes a relay 10, an electrical connector 11, a temperature control instrument 9, and a temperature sensor 20; the relay 10 is arranged in the casing 1 and the upper cover plate 2 connected to form a hollow cavity; the temperature The control instrument 9 is arranged on the front panel of the housing 1 for controlling and displaying the temperature; the electrical connector 11 is arranged at the bottom of the bottom cavity 3 for the connection of lines and the sealing of the bottom cavity 3 . The heating rod 16 and the temperature sensor 20 are arranged on the heating column 19; preferably, the relay 10 is a solid state relay, and the solid state relay is installed on the rear panel of the housing 1 to assist the temperature control instrument 9 to control the heating rod 16; preferably Ground, the electrical connector 11 is an aviation plug.

In another preferred example, the device for heating thermoplastic samples includes a relay 10, an electrical connector 11, a temperature control instrument 9, a temperature sensor 20, and a heating rod 16; the heating column 19 is connected to the heating rod 16, and the heating column 19 is connected to the temperature sensor 20; the temperature control instrument 9 is connected to the temperature sensor 20 through the electrical connector 11; the relay output end of the temperature control instrument 9 is connected to the control signal input end of the relay 10; in the output circuit of the controlled system of the relay 10, the relay One pole of the load output end of 10 is connected to the positive pole of the power supply, the other pole is connected to one end of the heating rod 16 through the electrical connector 11, and the other end of the heating rod 16 is connected to the negative pole of the power supply through the electrical connector 11 to form a series circuit; the relay 10 is set The casing 1 and the upper cover 2 are connected to form a hollow cavity; the temperature control instrument 9 is arranged on the front panel of the casing 1 , and the electrical connector 11 is arranged at the bottom of the bottom cavity 3 . The input power supply of the temperature control instrument and the power supply of the load output terminal of the relay are the same power supply. Principle: After the device is powered on, the temperature control instrument 9 controls the relay 10 according to the comparison result between the temperature value detected and returned by the temperature sensor 20 and the temperature value set by the temperature control instrument 9 . When the returned temperature value is lower than the set value, the temperature control instrument 9 controls the relay 10 to close, so that the heating rod 16 is powered on and heated; when the return value is lower than the set value, the temperature control instrument 9 controls the relay 10 to turn off, so that It stops energizing the heating rod 16 . Further preferably, the relay 10 is a solid state relay. Further preferably, the electrical connector 11 is an aviation plug.

In a specific implementation, when mass spectrometry analysis is performed on a thermoplastic sample, the analyzed sample needs to be crushed in advance so as to be sufficiently heated. Take a clean crucible 18, and place an appropriate amount of the crushed sample inside the crucible 18 for use. Move the snap assembly 5, remove the upper top chamber 4, then clamp the crucible 18 containing the sample with crucible tongs, and place it in the corresponding groove of the heating column 19; install the upper top chamber 4, and pass the snap Assembly 5 is locked to ensure sealing. Before starting to heat the sample, the heating and airtight chamber formed by the upper top chamber 4 and the bottom chamber 3 needs to be evacuated with air to avoid the influence of the residue from the previous sample analysis on this experiment. Start the mass spectrometer and begin the mass spectrometer pump down process. At this time, a pressure difference will be formed at both ends of the capillary 6 connecting the mass spectrometer and the heating closed chamber, so that the air in the high pressure heating closed chamber flows out through the capillary 6 and is evacuated by the vacuum pump system of the mass spectrometer. Play the role of air evacuation. The evacuation is carried out for about 2 minutes, the power supply of the device for heating the thermoplastic sample is turned on, and corresponding settings are made on the temperature control instrument 9 according to the target temperature of the sample to be studied. Under the heating of the heating rod 16, the thermoplastic begins to pyrolyze, and the pyrolyzed gaseous substances enter the ionization source end of the mass spectrometer and are ionized under the pressure difference between the two ends of the capillary 6. After the experiment is completed, the crucible 18 needs to be removed and the sample residue disposed of. At the same time, when the upper top chamber 4 is opened, the heating column 19 is properly heated and maintained for 10 minutes to accelerate the volatilization of the residue adsorbed on the inner surface. After completion, turn off the power of the device for heating the thermoplastic sample, install the upper top chamber 4 and lock it to prevent the water vapor in the air from being adsorbed to the inner surface of the chamber and affect the next use.

In the description of this application, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", The orientation or positional relationship indicated by "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the accompanying drawings, which is only for the convenience of describing the present application and simplifying the description, rather than indicating or implying the indicated device. Or elements must have a particular orientation, be constructed and operate in a particular orientation, and therefore should not be construed as a limitation of the present application.

The specific embodiments of the present invention have been described above. It should be understood that the present invention is not limited to the above-mentioned specific embodiments, and those skilled in the art can make various changes or modifications within the scope of the claims, which do not affect the essential content of the present invention. The embodiments of the present application and features in the embodiments may be combined with each other arbitrarily, provided that there is no conflict.

Claims (10)

1. a kind of device of heating thermoplastic plastic sample, which is characterized in that including shell (1), upper cover plate (2), bottom end chamber (3), top cavity (4), heated beam (19)；

Shell (1), upper cover plate (2) connection form hollow cavity；

Bottom end chamber (3) setting is above upper cover plate (2), and top cavity (4) setting is above bottom end chamber (3), bottom end chamber (3) He Shangding Chamber (4) is detachably connected or is flexibly connected；Top cavity (4) has exhaust outlet (22), and the chamber of top cavity (4) passes through exhaust outlet (22) connection is external；

Heated beam (19) is arranged in the cavity that bottom end chamber (3) and top cavity (4) are collectively formed, and heated beam is provided with sample on (19) Product containing groove；Heated beam (19) and bottom end chamber (3) fastening are installed, and are deposited between the notch and exhaust outlet (22) of sample containing groove In gap.

2. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that including heating rod (16), The heating rod (16) is arranged on heated beam (19).

3. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that the bottom end chamber (3) and Top cavity (4) is connected by snap component (5).

4. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that including crucible (18), add One end of plume (19) be provided with the crucible (18) matched groove, the other end of heated beam (19) is provided with and heating rod (16) matched mounting hole and with temperature sensor (20) matched mounting hole.

5. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that including the first sealing ring (15), the second sealing ring (17), interface flange (8)；

Interface flange (8) is mounted on the upper top cover of top cavity (4)；

Top cavity (4) is tightly connected by the first sealing ring (15) and bottom end chamber (3)；

Top cavity (4) is tightly connected by the second sealing ring (17) and interface flange (8).

6. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that including interior heat-insulating shield (14), outer heat-insulating shield (13)；

Heated beam (19) is installed in bottom end chamber (3) by interior heat-insulating shield (14)；

Shell (1) is mounted on bottom end chamber (3) bottom by outer heat-insulating shield (13).

7. the device of heating thermoplastic plastic sample according to claim 5, which is characterized in that including connecting tube (6)；

Connecting tube (6) and interface flange (8) airtight connection, connecting tube (6) are connected to exhaust outlet (22)；The connecting tube (6) is hair Tubule.

8. the device of heating thermoplastic plastic sample according to claim 7, which is characterized in that including pipe adapter (7)； Pipe adapter (7) one end connects connecting tube (6) by interface flange (8) connection exhaust outlet (22), the other end.

9. the device of heating thermoplastic plastic sample according to claim 7, which is characterized in that the chamber of bottom end chamber (3) It is mutually isolated between the chamber of top cavity (4).

10. the device of heating thermoplastic plastic sample according to claim 1, which is characterized in that including relay (10), Electric connector (11), temperature controller device (9), temperature sensor (20), heating rod (16)；

Heated beam (19) is connect with heating rod (16), and heated beam (19) is connect with temperature sensor (20)；

Temperature controller device (9) passes through electric connector (11) connection temperature sensor (20)；The relay of temperature controller device (9) Output end connects the control signal input of relay (10)；In relay (10) by control system output loop, relay One pole of the load outputs of device (10) is connected with positive pole, and another pole passes through electric connector (11) connection heating rod (16) The other end of one end, heating rod (16) is connected by electric connector (11) with power cathode；

Relay (10) setting is formed in hollow cavity in shell (1), upper cover plate (2) connection；

Temperature controller device (9) is arranged on shell (1) front panel, and electric connector (11) is arranged in bottom end chamber (3) bottom.