CN107228789B - Thermal cracker with temperature measurement function and mercury analyzer - Google Patents
Thermal cracker with temperature measurement function and mercury analyzer Download PDFInfo
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- CN107228789B CN107228789B CN201710639698.5A CN201710639698A CN107228789B CN 107228789 B CN107228789 B CN 107228789B CN 201710639698 A CN201710639698 A CN 201710639698A CN 107228789 B CN107228789 B CN 107228789B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The thermal cracker with the temperature measuring function comprises a cracking reaction container, a heating device, a reference container, a temperature measuring device and a temperature measuring device, wherein the structure and the working temperature of the reference container are the same as those of the cracking reaction container; the temperature measuring device is a temperature measuring instrument or a temperature measuring probe arranged in the reference container. According to the invention, the cracking reaction container and the reference container with the same structure and the same working environment are arranged at the same time, so that the cracking reaction container and the reference container always have the same working temperature, and the actual working temperature in the cracking reaction container can be obtained by measuring the internal temperature of the reference container, thereby providing a reference for realizing the temperature control of the experimental substance decomposition reaction. The thermal cracker is applied to the mercury analyzer, so that the temperature control precision of the mercury analyzer in a cracking reaction link can be realized, and meanwhile, the external impurity interference caused by temperature measurement can be avoided, thereby improving the measurement accuracy and measurement precision of the mercury analyzer.
Description
Technical Field
The invention belongs to the technical field of chemistry, and relates to a thermal cracker for carrying out thermal cracking reaction on a compound and a mercury analyzer for measuring mercury element in the compound.
Background
The thermal cracker is also called an atomizer, and functions to thermally crack an organic or inorganic form of an element to thereby atomize the element so as to analyze the component thereof by a detector. The operating temperature of the thermal cracker directly affects the degree of atomization of the test substance and thus further affects the accuracy with which the components are analyzed by the detector. It follows that the temperature control during operation of the thermal cracker is critical and that the measurement of temperature is the basic basis for implementing the temperature control.
The thermal cracker (for example, the chinese patent 200780036562X) adopted by the existing mercury analyzer generally has no temperature detecting device, and a worker generally can directly operate the external heating device only by experience, so that it is difficult to accurately measure and control the internal temperature of the reaction vessel of the thermal cracker. If a temperature measuring device is placed in the reaction vessel of the thermal cracker, the actual working temperature of the thermal cracker is directly measured, and the content of the detected element is usually very low (for example, the content of mercury in food, polluted water source or soil is detected), the metal or plastic packaging shell of the temperature measuring device can generate impurities and interfere with the cracking reaction of experimental gas due to the high temperature environment, so that the accuracy of experimental results is seriously affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the thermal cracker with the temperature measurement function, which has the advantages of simple structure, simple and convenient operation, high reliability and high accuracy of experimental results, and the mercury analyzer adopting the thermal cracker.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the thermal cracker with the temperature measuring function comprises a cracking reaction container, a heating device, a reference container, a temperature measuring device and a temperature measuring device, wherein the structure and the working temperature of the reference container are the same as those of the cracking reaction container; the temperature measuring device is a temperature measuring instrument arranged in the reference container or a temperature measuring probe of the temperature measuring instrument.
A mercury analyzer comprises an automatic sampler, an enrichment and desorption module, a separation and thermal cracking module and a detector which are connected in sequence; the separation and thermal cracking module employs a thermal cracker having a temperature measurement function as described above.
According to the thermal cracker with the temperature measurement function, the cracking reaction container and the reference container with the same structure and the same working environment are arranged at the same time, so that the cracking reaction container and the reference container always have the same working temperature, the actual working temperature in the cracking reaction container can be obtained by measuring the temperature in the reference container, and a reference is provided for realizing the temperature control of the decomposition reaction of experimental substances. The thermal cracker is applied to the mercury analyzer, so that the temperature control precision of the mercury analyzer in a cracking reaction link can be realized, and the external impurity interference cannot be introduced due to temperature measurement, thereby improving the measurement accuracy and measurement precision of the mercury analyzer.
Drawings
FIG. 1 is a schematic diagram of a thermal cracker with temperature measurement according to one embodiment of the present invention;
FIG. 2 is a schematic view showing the structure of another embodiment of a thermal cracker with temperature measuring function according to the present invention;
FIG. 3 is a schematic view showing the structure of a third embodiment of a thermal cracker with temperature measuring function according to the present invention;
FIG. 4 is a schematic cross-sectional view of a dual chamber quartz tube of a third embodiment of a thermal cracker with temperature measurement function according to the present invention;
fig. 5 is a schematic diagram showing the overall structure of a mercury analyzer according to the present invention.
Detailed Description
Embodiments of a thermal cracker and a mercury analyzer having a temperature measuring function according to the present invention are further described below with reference to examples and drawings. The thermal cracker with temperature measuring function and the mercury analyzer according to the present invention are not limited to the description of the following examples.
A thermal cracker with temperature measurement function comprises a cracking reaction container and a heating device; the device also comprises a reference container which has the same structure and working temperature as those of the cracking reaction container and is used for arranging a temperature measuring device. The temperature measuring device is a temperature measuring instrument arranged in the reference container or a temperature measuring probe of the temperature measuring instrument. The thermometer can directly adopt various products on the market, including but not limited to thermal resistance type, radiation type, spectrum type, ultrasonic type or laser type. The specific embodiment of the thermal cracker with the temperature measuring function is as follows.
Example 1
As shown in fig. 1, the pyrolysis reaction container and the reference container of the thermal cracker with temperature measuring function are a first quartz tube 11 and a second quartz tube 12 which are respectively identical in structure and are arranged side by side. The heating device is a first resistance wire 21, the first resistance wire 21 is uniformly wound outside a first quartz tube 11 and a second quartz tube 12 which are arranged side by side, and the first resistance wire 21 is electrified and heats to heat the first quartz tube 11 and the second quartz tube 12. Since the first quartz tube 11 and the second quartz tube 12 have the same structure, the same heating mode and the same heating area, the working temperatures inside the two quartz tubes are necessarily the same.
As another heating mode of the present embodiment, the heating device is a micro boiler, and similar effects can be achieved by arranging the first quartz tube 11 and the second quartz tube 12 in the micro boiler.
Example 2
As shown in fig. 2, the pyrolysis reaction vessel and the reference vessel of the thermal cracker with temperature measuring function are respectively a first quartz tube 11 and a second quartz tube 12 with the same structure, and a first resistance wire 21 and a second resistance wire 22 are respectively and uniformly wound on the outer parts of the two quartz tubes. The first resistance wire 21 and the second resistance wire 22 are identical in material, structure, length and winding manner, and the same resistance value is ensured. Thus, when the first and second resistance wires 21 and 22 pass the same current, they can generate the same heating effect, thereby realizing the same operating temperature inside the first and second quartz tubes 11 and 12.
Further, the first resistance wire 21 and the second resistance wire 22 are arranged in series, so that the same current is ensured, the complexity of current control is reduced, and the control precision is improved.
Example 3
As shown in fig. 3, the pyrolysis reaction container and the reference container of the thermal cracker with temperature measurement function are a first cavity 31 and a second cavity 32 of the dual-cavity quartz tube 3 respectively, the structures of the first cavity 31 and the second cavity 32 are the same or mirror image structures, and when the exterior of the dual-cavity quartz tube 3 is heated, the dual-cavity heating process and the working temperature can be ensured to be always the same. The heating device is a first resistance wire 21 uniformly wound outside the double-cavity quartz tube 3; alternatively, the heating device is a micro-boiler, and the double-cavity quartz tube 3 is arranged in the micro-boiler.
As shown in fig. 4, the section of the dual-cavity quartz tube 3 is in a shape of "θ", a shape of "8" or a shape of "ri", and may have the same or mirror image structure of the other two cavities.
Example 4
Referring to the above embodiments 1 to 3, the cleavage reaction vessel is used for passing the test gas, and the reference vessel is used for passing the reference gas having the same initial temperature and flow rate as those of the test gas, thereby ensuring that the low-temperature gas flow has the same cooling effect on the high-temperature cleavage reaction vessel and the reference vessel, so as to ensure that the cleavage reaction vessel and the reference vessel always have the identical working temperature. Further, the main components of the reference gas and the experimental gas are the same, or the components of the reference gas and the experimental gas are the same, so that the difference of cooling effects caused by the difference of specific heat capacities of the reference gas and the experimental gas is reduced.
Example 5
This example shows a specific embodiment of applying the thermal cracker with temperature measurement function described in examples 1 to 4 to mercury analysis.
The working temperature range of the thermal cracker is 700-900 ℃, and various forms of derivative compounds of mercury are blown into the thermal cracker through Ar gas to carry out thermal cracking reaction, so that the atomization of the mercury in various forms is realized.
Example 6
As shown in fig. 5, a mercury analyzer comprises an autosampler 1, an enrichment and desorption module 2, a separation and thermal cracking module 3 and a detector 4 which are connected in sequence; the separation and thermal cracking module 3 employs a thermal cracker having a temperature measurement function as described in examples 1 to 5.
The automatic sampler 1 integrates a purging function and comprises a first gas source 11, a sampling needle 12 and a sample bottle 13. The first gas source may be nitrogen, and is used for purging the sample solution entering the sample bottle 13 through the sample injection needle 12, and purging and separating volatile substances containing mercury elements in the sample bottle 13, and entering the enrichment and desorption module 2.
The enrichment and desorption module 2 includes a Tenax-rich pipe 21, a heater and an electromagnetic six-way valve 22, 1 each of which are provided for enriching, drying and desorbing volatile substances purged from the auto-injector 1 integrating the purge function. A second gas source 23 may be provided, generally leading from said electromagnetic six-way valve 22.
The separation and thermal cracking module 3 includes a gas chromatography separation column 31, a thermal cracker 32, and the gas chromatography separation column 31 is used for separating the volatile substances desorbed from the enrichment and desorption module 2 into single volatile substances, and thermally cracking the single volatile substances into atomic form mercury elements through the thermal cracker 32. The thermal cracker 32 of the separation and thermal cracking module 3 adopts the thermal cracker having the temperature measuring function as described in embodiments 1 to 5, so that the temperature measurement and control accuracy of the mercury analyzer in the cleavage reaction section can be achieved, thereby improving the measurement accuracy and measurement precision of the mercury analyzer.
The detector 4 comprises a light source, a flow cell and a photomultiplier tube, and is used for irradiating the atomic mercury from the separation and thermal cracking module 3 passing through the flow cell through the light source to excite the atomic mercury to a high energy state and then radiate resonance fluorescence when returning to a ground state, and obtaining the mercury content therein through photoelectric conversion and data processing and the amplified resonance fluorescence, thereby obtaining the alkyl mercury content
It should be noted that, the various quartz tubes used in embodiments 1 to 6 may be straight tube structures, or may be shaped structures such as "U", "S", and spiral structures, so as to improve heating efficiency, or may be conveniently placed in a micro boiler.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (2)
1. The utility model provides a thermal cracker with temperature measurement function, includes pyrolysis reaction container and heating device, its characterized in that: also comprises a reference container which has the same structure and working temperature as those of the cracking reaction container and is used for arranging a temperature measuring device,
the cracking reaction container and the reference container are respectively a first quartz tube and a second quartz tube with the same structure, the first quartz tube and the second quartz tube are arranged side by side and are jointly wound in a first resistance wire, the first resistance wire is uniformly wound outside the first quartz tube and the second quartz tube which are arranged side by side, and the first quartz tube and the second quartz tube are heated by electrifying and heating the first resistance wire; or the heating device is a first resistance wire which is wound outside the first quartz tube; the first resistance wire and the second resistance wire are in the same structure and are wound outside the second quartz tube, the working current of the first resistance wire and the working current of the second resistance wire are the same, the first resistance wire and the second resistance wire are arranged in series,
the cracking reaction container is used for passing through experimental gas, the reference container is used for passing through reference gas with the same initial temperature and flow rate as the experimental gas, and the reference gas and the experimental gas have the same components, so that the cracking reaction container and the reference container always have the same working temperature;
the cracking reaction container and the reference container of the thermal cracker with the temperature measurement function are a first containing cavity and a second containing cavity of the double-cavity quartz tube respectively, the structures of the first containing cavity and the second containing cavity are the same or mirror image structures, and when the outside of the double-cavity quartz tube is heated, the temperature rising process and the working temperature of the first containing cavity and the second containing cavity are always the same;
the working temperature range of the thermal cracker is 700-900 ℃, and various forms of derivative compounds of mercury are blown into the thermal cracker through Ar gas to carry out thermal cracking reaction, so that the atomization of various forms of mercury is realized;
the temperature measuring device is a temperature measuring instrument arranged in the reference container or a temperature measuring probe of the temperature measuring instrument.
2. The utility model provides a mercury analyzer, includes autosampler, enrichment and desorption module, separation and thermal cracking module, and detector that connect gradually, its characterized in that: the separation and thermal cracking module employs the thermal cracker with temperature measurement function as defined in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710639698.5A CN107228789B (en) | 2017-07-31 | 2017-07-31 | Thermal cracker with temperature measurement function and mercury analyzer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710639698.5A CN107228789B (en) | 2017-07-31 | 2017-07-31 | Thermal cracker with temperature measurement function and mercury analyzer |
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| CN107228789A CN107228789A (en) | 2017-10-03 |
| CN107228789B true CN107228789B (en) | 2023-09-08 |
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Citations (7)
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| JP2004184253A (en) * | 2002-12-04 | 2004-07-02 | Hitachi Plant Eng & Constr Co Ltd | Method for measuring organic volatile substance of organic material |
| CN101799439A (en) * | 2009-02-03 | 2010-08-11 | 梅特勒-托利多公开股份有限公司 | Thermo-analytical instrument |
| CN102192959A (en) * | 2010-03-11 | 2011-09-21 | 上海市计算技术研究所 | Thermal cracker, thermal cracking gas chromatograph and thermal cracking analysis method |
| CN102498376A (en) * | 2009-07-07 | 2012-06-13 | 弗兰克·列伊·吴 | A differential adiabatic compensation calorimeter and methods of operation |
| CN106644664A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Thermal desorption-gas phase separation-thermal pyrolysis system based on phenylated derived organic mercury |
| CN207300703U (en) * | 2017-07-31 | 2018-05-01 | 郝东辉 | A kind of heat cracker with temperature measurement function and a kind of mercury analyzer |
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2017
- 2017-07-31 CN CN201710639698.5A patent/CN107228789B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4195061A (en) * | 1977-05-17 | 1980-03-25 | Firma Vereinigte Edelstahlwerke Aktiengesellschaft | Sterilization apparatus for infusion solutions or the like, filled in containers |
| JP2004184253A (en) * | 2002-12-04 | 2004-07-02 | Hitachi Plant Eng & Constr Co Ltd | Method for measuring organic volatile substance of organic material |
| CN101799439A (en) * | 2009-02-03 | 2010-08-11 | 梅特勒-托利多公开股份有限公司 | Thermo-analytical instrument |
| CN102498376A (en) * | 2009-07-07 | 2012-06-13 | 弗兰克·列伊·吴 | A differential adiabatic compensation calorimeter and methods of operation |
| CN104807854A (en) * | 2009-07-07 | 2015-07-29 | 吴耿 | Heat system and operation method |
| CN102192959A (en) * | 2010-03-11 | 2011-09-21 | 上海市计算技术研究所 | Thermal cracker, thermal cracking gas chromatograph and thermal cracking analysis method |
| CN106644664A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Thermal desorption-gas phase separation-thermal pyrolysis system based on phenylated derived organic mercury |
| CN207300703U (en) * | 2017-07-31 | 2018-05-01 | 郝东辉 | A kind of heat cracker with temperature measurement function and a kind of mercury analyzer |
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| CN107228789A (en) | 2017-10-03 |
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