CN111220560A - Carbon nitrogen sulphur measuring equipment - Google Patents

Carbon nitrogen sulphur measuring equipment Download PDF

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Publication number
CN111220560A
CN111220560A CN202010221036.8A CN202010221036A CN111220560A CN 111220560 A CN111220560 A CN 111220560A CN 202010221036 A CN202010221036 A CN 202010221036A CN 111220560 A CN111220560 A CN 111220560A
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CN
China
Prior art keywords
gas
nitrogen
carbon
sulfur
purging
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Pending
Application number
CN202010221036.8A
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Chinese (zh)
Inventor
康希平
徐开群
何彬
罗建文
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Changsha Kaiyuan Instruments Co Ltd
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Changsha Kaiyuan Instruments Co Ltd
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Application filed by Changsha Kaiyuan Instruments Co Ltd filed Critical Changsha Kaiyuan Instruments Co Ltd
Priority to CN202010221036.8A priority Critical patent/CN111220560A/en
Publication of CN111220560A publication Critical patent/CN111220560A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/18Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity

Abstract

The invention discloses a carbon, nitrogen and sulfur measuring device which comprises a furnace body and a sleeve pipe assembly arranged in the furnace body, extending along the horizontal direction and used for placing a measuring vessel, wherein a heating element sleeved on the periphery of the sleeve pipe assembly and used for heating a sample is further arranged in the furnace body. The carbon, nitrogen and sulfur determination equipment is provided with a sleeve pipe assembly along the horizontal direction, and when a sample is detected, a measuring vessel with a sample is placed into the sleeve pipe assembly along the horizontal direction. The heating element burns the sample by heating the sample, and residue generated by the burning of the sample remains in the measuring vessel. The detector takes out the measuring vessel along the horizontal direction, and then the residue can be detected.

Description

Carbon nitrogen sulphur measuring equipment
Technical Field
The invention relates to the technical field of measuring instruments, in particular to a carbon, nitrogen and sulfur measuring device.
Background
Carbon and sulfur are mainly measured by an infrared spectrum absorption method, and specifically, sulfur and carbon elements are qualitatively and quantitatively analyzed by utilizing the selective absorption characteristics of gases such as SO2 and CO2 to infrared light. In the detection of an actual instrument, substances are combusted and decomposed in oxygen flow at high temperature, gas generated by combustion passes through an infrared detection cell after being filtered, and the content of carbon and sulfur in coal is calculated by converting the gas concentration into a voltage signal through a circuit according to the Lambert beer law by utilizing the characteristic of selective absorption of the gas to infrared light.
There are two main methods for measuring nitrogen: kjeldahl method and dumas combustion method. At present, in the food industry, the Kjeldahl method is a commonly used method for detecting the content of crude protein; however, organic matter, particularly nitrate-containing samples, are difficult to convert quantitatively to ammonia and thus can severely affect the overall nitrogen results. The dumas combustion method has no problems, and has the advantages of rapidness, accuracy, no pollution and the like, so that the dumas combustion method is adopted in more and more fields.
The Dumas combustion method is that a sample is combusted at a high temperature of 900-1200 ℃, mixed gas is generated in the combustion process, interference components in the mixed gas are absorbed by a series of proper absorbents, nitrogen oxides in the mixed gas are completely reduced into molecular nitrogen, and then the content of the nitrogen is detected by a thermal conductivity detector.
Because need completely cut off the nitrogen gas in the air before the burning, so the nitrogen measuring appearance that current adopted the dumas combustion method all adopts vertical furnace structure basically, and the sample uses tin paper cup to wrap up sealed, makes things convenient for the sample to freely fall into or fall into furnace by the air-blast. The sample amount which can be tested by the method is usually small due to the sizes of the tinfoil cup and the sample dropping opening, and after the test is finished, residues are directly discarded and fall to the bottom of a hearth, so that the residues (such as cellulose and the like) cannot be quantitatively analyzed.
Therefore, how to provide a carbon, nitrogen and sulfur measuring device which is convenient for collecting the burned residues is a technical problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a carbon, nitrogen and sulfur measuring device, wherein a sleeve assembly of the device extends along the horizontal direction, so that a measuring vessel can be conveniently put in and taken out, and further, the purpose of taking out residues generated after combustion is realized.
In order to achieve the above purpose, the present invention provides a carbon, nitrogen and sulfur measuring apparatus, which comprises a furnace body and a sleeve assembly arranged in the furnace body, extending along a horizontal direction, for placing a measuring vessel, wherein a heating element sleeved on the outer periphery of the sleeve assembly and used for heating a sample is further arranged in the furnace body.
Preferably, one end of the sleeve assembly is a closed end, the other end of the sleeve assembly is an open end, the closed end is inserted into the furnace body, the open end is suspended outside the furnace body, and the open end is provided with a furnace door for closing the sleeve assembly.
Preferably, the sleeve assembly is further connected with a purging mechanism for purging the interior of the sleeve assembly.
Preferably, the blowing mechanism comprises a blowing head connected with the open end, a blowing chamber communicated with the interior of the sleeve assembly is arranged in the blowing head, and a blowing pipe used for conveying blowing air is further arranged on the side wall of the blowing head.
Preferably, one end of the blowing head, which is far away from the sleeve component, is provided with a blowing door, and the furnace door is positioned between the open end and the blowing head.
Preferably, the gas path analysis mechanism is connected with the sleeve assembly and used for analyzing gas generated by sample combustion.
Preferably, the gas path analysis mechanism comprises a gas blowing pipe arranged in the blowing head and used for conveying oxygen to the sample and a gas collecting head used for extracting gas generated by combustion, the gas blowing pipe is connected with a gas source, and the gas collecting head is connected with the measuring device.
Preferably, the sleeve assembly comprises an inner corundum tube and an outer corundum tube which are coaxially arranged, the opening end is provided with a gas collection chamber, the gas collection head is installed in the gas collection chamber, a flow channel which is communicated with the inner side of the inner corundum tube and used for gas generated by combustion is arranged between the inner corundum tube and the outer corundum tube, and the gas collection head is communicated with the flow channel.
Preferably, a drying pipe for drying gas generated by combustion and a filter for filtering solid particles are further arranged in the gas path analysis mechanism, and the filter is located at an inlet of the vacuum pump.
Preferably, the outlet of the vacuum pump is connected with a gas mixing tank, the gas path analysis mechanism further comprises a quantitative sampler connected with the gas mixing tank and used for extracting a gas sample, the quantitative sampler is connected with the inlet of the reduction furnace, and the outlet of the reduction furnace is connected with the measuring device.
The carbon, nitrogen and sulfur measuring equipment provided by the invention comprises a furnace body and a sleeve pipe assembly which is arranged in the furnace body, extends along the horizontal direction and is used for placing a measuring vessel, and a heating element which is sleeved on the periphery of the sleeve pipe assembly and is used for heating a sample is also arranged in the furnace body.
The carbon, nitrogen and sulfur determination equipment is provided with a sleeve pipe assembly along the horizontal direction, and when a sample is detected, a measuring vessel with a sample is placed into the sleeve pipe assembly along the horizontal direction. The heating element burns the sample by heating the sample, and residue generated by the burning of the sample remains in the measuring vessel. The detector takes out the measuring vessel along the horizontal direction, and then the residue can be detected.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural view of a carbon, nitrogen and sulfur measuring apparatus according to the present invention;
FIG. 2 is a schematic view of the structure of the cleaning head of FIG. 1;
FIG. 3 is a schematic structural view of a gas path analyzing mechanism in the carbon, nitrogen and sulfur measuring apparatus.
Wherein the reference numerals in fig. 1 to 3 are:
the device comprises a measuring vessel 1, an air blowing pipe 2, a furnace mouth plate 3, an air collecting chamber 4, an outer corundum pipe 5, a furnace body 6, an inner corundum pipe 7, a heating element 8, an air collecting head 9, a furnace door 10, a blowing head 11, a blowing door 12, a blowing pipe 13, a blowing outlet 14, an oxygen gas source 15, a carrier gas source 16, a flow meter 17, a drying pipe 18, a filter 19, a vacuum pump 20, a gas mixing tank 21, a quantitative sampler 22, a reduction furnace 23, a flow stabilizer 24, a carbon infrared pool 25, a sulfur infrared pool 26, a purifier 27 and a heat conducting pool 28.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order that those skilled in the art will better understand the disclosure, the invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1 to 3, fig. 1 is a schematic structural diagram of a carbon, nitrogen and sulfur measuring apparatus provided by the present invention; FIG. 2 is a schematic view of the structure of the cleaning head of FIG. 1; FIG. 3 is a schematic structural view of a gas path analyzing mechanism in the carbon, nitrogen and sulfur measuring apparatus.
The carbon, nitrogen and sulfur measuring equipment provided by the invention comprises a furnace body 6 and a heating element 8. As shown in fig. 1, one end of the sleeve assembly is a closed end, and the other end is an open end, wherein the closed end is inserted into the furnace body 6 along the horizontal direction, and the open end is suspended outside the furnace body 6. The heating element 8 is arranged in the furnace body 6 and sleeved on the periphery of the sleeve pipe assembly. The heating element 8 may be embodied as a tubular electric heater or a heating coil, etc., and the heating element 8 is used for heating the sleeve assembly so as to heat the sample to be burned in the sleeve assembly. In the measuring process, a tester places a sample in a measuring vessel 1 such as a quartz crucible or a ceramic crucible, the sample is arranged in a furnace body 6 in a combined mode through tools such as a sample feeding rod, the sample generates sulfur dioxide, carbon dioxide and nitrogen oxide after being heated and combusted, the carbon nitrogen sulfur measuring equipment further comprises a detecting component for detecting sulfur, carbon and nitrogen, the detecting component extracts gas generated by combustion, and the content of three elements in the sample is determined through the content of sulfur, carbon and nitrogen in the detecting gas.
Optionally, in order to avoid air influence on the measurement result, the open end is further provided with an oven door 10, the oven door 10 is opened to place the sample into the sleeve assembly before detection, and then the oven door 10 is closed to seal the interior of the sleeve assembly. The structure of the detecting component can refer to the prior art, and is not described in detail herein.
Furthermore, the sleeve assembly is also connected with a purging mechanism for purging the interior of the sleeve assembly. The purging mechanism is connected with a carrier gas source 16, the carrier gas is usually a gas which does not react with the sample, and certainly does not contain three elements of sulfur, carbon and nitrogen, so that the measurement result is prevented from being influenced. As shown in fig. 3, the input of the carrier gas is controlled by a solenoid valve, and the carrier gas enters the sleeve assembly for purging after being filtered and stabilized.
Optionally, the open end is provided with a furnace mouth plate 3, the purging mechanism comprises a tubular purging head 11, the purging head 11 and the side surface of the furnace mouth plate 3 far away from the furnace body 6 are fixedly connected, and the purging head 11 and the sleeve assembly are coaxially arranged. The purge head 11 forms a purge chamber, as shown in fig. 2, one side of the purge chamber is provided with a purge tube 13, the other side is provided with a purge outlet 14, the carrier gas is blown into the sleeve assembly through the purge tube 13 and discharged through the purge outlet 14, and the gas in the sleeve assembly is replaced by the carrier gas. In addition, in order to avoid carrier gas leakage in the purging process, one end, far away from the furnace body 6, of the purging head 11 is provided with a purging door 12, and the purging door 12 can seal the purging chamber to ensure that the carrier gas flows out from the purging outlet 14. In addition, during the measurement process, the furnace door 10 and the purging door 12 are closed simultaneously, so that the sealing performance of the sleeve assembly can be improved.
In this embodiment, carbon nitrogen sulphur survey equipment sets up the thimble assembly along the horizontal direction, adopts horizontal furnace can conveniently measure household utensils 1 and put into and take out the thimble assembly, and can carry out quantitative analysis to the residue after taking out the measurement household utensils 1 that will have the residue, improves the accuracy of survey. In addition, the sleeve assembly is connected with a component such as a purge head 11, the component can replace the gas in the sleeve assembly out of the sleeve assembly, and the purge head 11 can seal the sleeve assembly in the measuring process, so that the sealing performance of the carbon-nitrogen-sulfur measuring equipment is improved.
Optionally, the carbon, nitrogen and sulfur measuring equipment further comprises a gas path analysis mechanism, and the gas path analysis mechanism is connected with the sleeve assembly. After the sample burns to generate gas, the gas path analysis mechanism extracts the gas in the sleeve assembly and analyzes the gas.
Optionally, the gas path analyzing mechanism includes a gas collecting head 9 and a measuring device. As shown in fig. 1, the sleeve assembly comprises an inner alundum tube 7 and an outer alundum tube 5 which are coaxially arranged, and the measuring vessel 1 is placed in the inner alundum tube 7 in the measuring process to form a flow passage for flowing gas generated by combustion. One side of the furnace mouth plate 3 facing the furnace body 6 is provided with a gas collection chamber 4, an opening of the flow channel is positioned in the gas collection chamber 4, a gas collection head 9 is arranged in the gas collection chamber 4, and a gas path analysis mechanism can generate negative pressure, so that gas generated by combustion flows into the measuring device through the flow channel and the gas collection head 9.
Further, the carbon nitrogen sulfur measuring equipment is also provided with an air blowing pipe 2, as shown in fig. 1 and fig. 2, the air blowing pipe 2 is arranged in the blowing head 11 and extends to the bottom of the sleeve assembly along the axial direction, the air blowing pipe 2 is connected with an oxygen source 15, oxygen is blown into the sleeve assembly by the air blowing pipe 2, and combustion supporting effect is achieved in the measuring process. As shown in figure 3, a filter 19, a voltage stabilizer and an electromagnetic valve are also arranged between the oxygen gas source 15 and the gas blowing pipe 2, and the carbon, nitrogen and sulfur measuring equipment controls the input amount of oxygen through the electromagnetic valve. In addition, the carbon nitrogen sulfur measuring device is also provided with a flow meter 17 for measuring the oxygen flow rate, so that the oxygen input amount can be conveniently calculated during measurement.
Optionally, the gas path analyzing mechanism comprises a vacuum pump 20, and the vacuum pump 20 is used for extracting gas generated by combustion. The inlet of the vacuum pump 20 is provided with a drying pipe 18 and a filter 19, the moisture generated by the combustion of the sample is absorbed by the drying pipe 18, the solid particles are filtered by the filter 19, and the clean gas flows into the vacuum pump 20, so that the service life of the vacuum pump 20 can be prolonged, and the accuracy of the measurement can be improved.
Further, the outlet of the vacuum pump 20 is connected with a gas mixing tank 21, and gas flows into the gas mixing tank 21 for buffering, so that the stability of the gas pressure is ensured. The gas path analyzing mechanism further includes a quantitative sampler 22, and the quantitative sampler 22 extracts a quantitative gas from the gas mixture tank 21 for measurement. The outlet of the quantitative sampler 22 is connected to the inlet of the reduction furnace 23, and the nitrogen oxides are reduced to nitrogen molecules in the reduction furnace 23. The outlet of the reduction furnace 23 is connected with a measuring device, the measuring device comprises a carbon infrared cell 25, a sulfur infrared cell 26 and a thermal conductivity cell, and the carbon infrared cell 25 and the sulfur infrared cell 26 respectively measure the content of carbon and sulfur in the gas by an infrared spectrum absorption method. The thermal conductivity cell 28 is used for detecting the content of nitrogen element, nitrogen oxide is generated after nitrogen in the sample is combusted, the nitrogen oxide enters the gas path analysis mechanism along with gas, a reduction furnace in the gas path analysis mechanism reduces the nitrogen oxide into nitrogen molecules, and the thermal conductivity cell 28 detects the content of the nitrogen molecules according to different thermal conductivities. In addition, in order to avoid the influence of carbon dioxide, sulfur dioxide and water molecules on the detection of the content of nitrogen molecules, a purifier 27 is further arranged in the gas path analysis mechanism, and an absorbent is arranged in the purifier 27 and can absorb the carbon dioxide, the sulfur dioxide and the water molecules. In addition, a flow stabilizer 24 is provided between the measuring device and the reduction furnace 23 in order to ensure a stable flow of the gas into the measuring device.
In this embodiment, the carbon, nitrogen and sulfur measuring device is provided with a special gas path analysis mechanism, the gas path analysis mechanism extracts gas generated by combustion through the vacuum pump 20, and measures the contents of three elements of sulfur, carbon and nitrogen through the measuring device.
It is noted that, in this specification, relational terms such as first and second, and the like are used solely to distinguish one entity from another entity without necessarily requiring or implying any actual such relationship or order between such entities.
The carbon, nitrogen and sulfur measuring equipment provided by the invention is described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (10)

1. The carbon, nitrogen and sulfur measuring equipment is characterized by comprising a furnace body (6) and a sleeve pipe assembly which is arranged in the furnace body (6), extends along the horizontal direction and is used for placing a measuring vessel (1), wherein a heating element (8) which is sleeved on the periphery of the sleeve pipe assembly and is used for heating a sample in the sleeve pipe assembly is further arranged in the furnace body (6).
2. The apparatus for carbon, nitrogen and sulfur determination according to claim 1, wherein one end of the sleeve assembly is a closed end, and the other end is an open end, the closed end is inserted into the furnace body (6), the open end is suspended outside the furnace body (6), and the open end is provided with a furnace door (10) for closing the sleeve assembly.
3. The apparatus for measuring carbon, nitrogen and sulfur as claimed in claim 2, wherein said sleeve assembly further comprises a purging mechanism for purging the interior thereof.
4. The carbon nitrogen sulfur measuring device according to claim 3, characterized in that the purging mechanism comprises a purging head (11) connected with the open end, the purging head (11) has therein a purging chamber communicating with the interior of the casing assembly, and a purging pipe (13) for conveying a purging air is further provided on a side wall of the purging head (11).
5. The carbon nitrogen sulfur measuring equipment according to the claim 4, characterized in that the end of the blowing head (11) far away from the sleeve component is provided with a blowing door (12), and the furnace door (10) is positioned between the open end and the blowing head (11).
6. The apparatus as claimed in any one of claims 3 to 5, further comprising a gas path analysis mechanism connected to the sleeve assembly for analyzing gas generated by combustion of the sample.
7. The carbon, nitrogen and sulfur measuring equipment as claimed in claim 6, wherein the gas path analyzing mechanism comprises a gas blowing pipe (2) arranged in the blowing head (11) and used for conveying oxygen to the sample and a gas collecting head (9) used for extracting gas generated by combustion, the gas blowing pipe (2) is connected with a gas source, and the gas collecting head (9) is connected with a measuring device.
8. The carbon nitrogen sulfur measuring device according to claim 7, characterized in that the sleeve assembly comprises an inner corundum tube (7) and an outer corundum tube (5) which are coaxially arranged, the open end is provided with a collection chamber (4), the gas collection head (9) is installed in the collection chamber (4), a flow passage which is communicated with the inner side of the inner corundum tube (7) and is used for combustion of generated gas is arranged between the inner corundum tube (7) and the outer corundum tube (5), and the gas collection head (9) is communicated with the flow passage.
9. The apparatus for measuring carbon, nitrogen and sulfur as claimed in claim 8, wherein said gas path analyzing means further comprises a drying tube (18) for drying the gas generated by combustion and a filter (19) for filtering solid particles, said filter (19) being located at the inlet of a vacuum pump (20).
10. The apparatus for measuring carbon, nitrogen and sulfur as claimed in claim 9, wherein the outlet of the vacuum pump (20) is connected to a gas mixing tank (21), the gas path analyzing mechanism further comprises a quantitative sampler (22) connected to the gas mixing tank (21) for extracting a gas sample, the quantitative sampler (22) is connected to the inlet of a reduction furnace (23), and the outlet of the reduction furnace (23) is connected to the measuring device.
CN202010221036.8A 2020-03-25 2020-03-25 Carbon nitrogen sulphur measuring equipment Pending CN111220560A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010221036.8A CN111220560A (en) 2020-03-25 2020-03-25 Carbon nitrogen sulphur measuring equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010221036.8A CN111220560A (en) 2020-03-25 2020-03-25 Carbon nitrogen sulphur measuring equipment

Publications (1)

Publication Number Publication Date
CN111220560A true CN111220560A (en) 2020-06-02

Family

ID=70830115

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010221036.8A Pending CN111220560A (en) 2020-03-25 2020-03-25 Carbon nitrogen sulphur measuring equipment

Country Status (1)

Country Link
CN (1) CN111220560A (en)

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