CN212341012U - Miniaturized detection device of tin content based on atomic emission spectroscopy - Google Patents

Miniaturized detection device of tin content based on atomic emission spectroscopy Download PDF

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Publication number
CN212341012U
CN212341012U CN202020191949.5U CN202020191949U CN212341012U CN 212341012 U CN212341012 U CN 212341012U CN 202020191949 U CN202020191949 U CN 202020191949U CN 212341012 U CN212341012 U CN 212341012U
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China
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liquid
way valve
passageway
gas
tubular reactor
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CN202020191949.5U
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Chinese (zh)
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陈丽霞
许丽建
许环军
张晓琳
王根
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Qiongtai Normal University
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Qiongtai Normal University
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Abstract

The utility model discloses a miniaturized detection device of tin content based on atomic emission spectroscopy, including multichannel peristaltic pump and six-way valve, set up carrier liquid passageway and reaction liquid passageway on the multichannel peristaltic pump, wherein, the carrier liquid passageway is connected with the inlet of six-way valve, be equipped with the sample solution passageway on the introduction port of six-way valve, be equipped with mixed liquid outlet on the appearance mouth of six-way valve, it is linked together with the reaction liquid passageway to mix liquid outlet, the other end and the tubular reactor of mixed liquid outlet are connected, set up the heater on the tubular reactor, tubular reactor's liquid outlet passes through the pipeline and is connected with vapour and liquid separator's inlet, vapour and liquid separator's air inlet and carrier gas pipeline are connected, vapour and liquid separator's gas outlet is passed through the pipeline and is connected with the air inlet of desicator, the gas outlet of desicat. The utility model discloses a tin content detection device's miniaturization, energy consumption are few, easy operation.

Description

Miniaturized detection device of tin content based on atomic emission spectroscopy
Technical Field
The utility model belongs to a chemical analysis field relates to a tin content detection device, specifically is a miniaturized device of tin content detection based on hydride takes place-atomic emission spectroscopy.
Background
Tin is a low melting metal element with a bluish white luster, which is not oxidized by air, and exists mainly in the form of dioxide (cassiterite) and various sulfides (e.g., thiocassiterite). Nowadays, tin and its compounds are widely used in pesticides, stabilizers, catalysts, additives, emulsifiers for ceramics industry, etc., which may remain in foods and medicines by contact with packaging materials, improper use, etc. Excessive intake of tin and its compounds can cause dizziness, diarrhea, nausea, chest distress, tachypnea, and reduction of calcium content in blood serum, which can cause gastroenteritis, and in severe cases, can cause damage to nervous system, liver function, skin mucosa, etc.
The limit value of tin in food is 250mg kg-1, the limit value of tin in beverage is 150mg kg-1, and the limit value of tin in infant formula food and infant auxiliary food is 50mg kg-1. In order to ensure that the tin content in food and medicine meets the national standard, China develops various methods for measuring the tin content.
In the determination of tin in food safety national standard food (GB 5009.16-2014), the first method selects atomic fluorescence spectroscopy for hydrogenation, which is based on the principle that a sample is digested by heating with acid, tin is oxidized to tetravalent tin, tin hydride is generated under the action of sodium borohydride and carried into an atomizer by a carrier gas for atomization, ground-state tin atoms are excited to a high energy state under the irradiation of a special tin hollow cathode lamp, and fluorescence with characteristic wavelength is emitted when the ground-state tin atoms are deactivated and returned to the ground state, and the fluorescence intensity is proportional to the tin content. The second method selects a lumefantrine colorimetric method, and the principle is that after a sample is digested, tetravalent tin ions and lumefantrine form a slightly soluble orange-red complex in a weakly acidic solution, and the slightly soluble orange-red complex is compared and quantified with a standard series solution in the presence of protective colloid. The classical methods have high accuracy and good stability, but the used instruments are large, the energy consumption is high, the operation is complex, and certain inconvenience is caused to the detection of the tin content in foods and medicines in the field and on site.
SUMMERY OF THE UTILITY MODEL
The utility model aims at not enough and provide a miniaturized detection device of tin content based on atomic emission spectrum to the little plasma in the glow discharge device makes tin atomic emission spectrum signal as the excitation source, according to its signal strength and the proportional linear relation of the concentration of tin, realizes the detection of tin content according to signal strength, has realized detection device's miniaturization, energy consumption are few, easy operation.
In order to accomplish the above object, the utility model adopts the following technical scheme:
the utility model provides a miniaturized detection device of tin content based on atomic emission spectroscopy, including multichannel peristaltic pump and six-way valve, set up carrier liquid passageway (hydrochloric acid carrier liquid) and reaction liquid passageway (sodium borohydride solution) on the multichannel peristaltic pump, wherein, the carrier liquid passageway is connected with the inlet of six-way valve, be equipped with the sample solution passageway on the introduction port of six-way valve, be equipped with mixed liquid eduction tube on the appearance mouth of six-way valve, the sample solution of following sample solution passageway input mixes in the six-way valve with the hydrochloric acid carrier liquid of carrier liquid passageway input (accurate ration of sample solution, operation such as mixing with hydrochloric acid carrier liquid can all be accomplished through the six-way valve operation), mixed liquid after the mixing flows out from mixed liquid eduction tube again, eduction tube and reaction liquid passageway mixed liquid are linked together, the other end of mixed liquid eduction tube is connected with tubular reactor, set up the heater on the tubular reactor, the mixed liquid (hydrochloric acid and carrier liquid solution) that flows out through mixed Reaction liquid (sodium borohydride solution) flowing from a liquid channel enters a tubular reactor after being mixed and reacts under the heating action of a heater, a liquid outlet of the tubular reactor is connected with a liquid inlet of a gas-liquid separator through a pipeline, a gas inlet of the gas-liquid separator is connected with a carrier gas pipeline, the reaction liquid after reaction enters the gas-liquid separator to separate gas from liquid, the separated gas is mixed with carrier gas (discharge gas) input from the carrier gas pipeline and flows out from a gas outlet above the gas-liquid separator along with the carrier gas, the remaining liquid flows out from a waste liquid outlet, a gas outlet of the gas-liquid separator is connected with a gas inlet of a drier through a pipeline, the mixed gas entering the drier is further dried, a gas outlet of the drier is connected with a glow discharge device through a pipeline, the dried mixed gas enters a glow discharge device and is excited to generate an emission spectrum, the method comprises the steps of collecting tin atom emission spectrum signals by using a spectrometer, comparing the tin atom emission spectrum signals in a sample solution to be detected by collecting tin atom emission spectrum signals in a standard solution because the intensity of the tin atom emission spectrum signals is in a linear relation with the tin content in the sample solution, and realizing quantitative detection of the tin content in the sample to be detected according to the signal intensity change.
According to the utility model discloses, it is preferred, tubular reactor designs for heliciform tubular reactor for mix the more even of liquid mixture.
According to the present invention, preferably, the heater is a microwave heater or an electric heater.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model discloses miniaturized detection device of tin content based on atomic emission spectroscopy to little plasma in the glow discharge device makes tin atomic emission spectroscopy signal as the excitation source, according to its signal strength and the proportional linear relation of the concentration of tin, realizes the detection of tin content according to signal strength, compares with traditional detection device, has realized detection device's miniaturization, energy consumption are few, easy operation.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Wherein: 1. a six-way valve; 2. a sample solution channel; 3. a multi-channel peristaltic pump; 4. a liquid carrying channel; 5. a reaction liquid channel; 6. a mixed liquid outlet pipe; 7. a tubular reactor; 8. a liquid inlet; 9. a gas-liquid separator; 10. a liquid outlet; 11. a carrier gas conduit; 12. an air outlet; 13. a dryer; 14. an exhaust gas vent; 15. a glow discharge device; 16. a CCD spectrometer; 17. a heater.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1, the utility model relates to a tin content miniaturized detection device based on atomic emission spectroscopy, including multichannel peristaltic pump 3 and six-way valve 1, set up carrier liquid passageway 4 and reaction liquid passageway 5 on the multichannel peristaltic pump 3, carrier liquid passageway 4 is the hydrochloric acid carrier liquid, reaction liquid passageway 5 is sodium borohydride reaction liquid, wherein, carrier liquid passageway 4 is connected with the inlet of six-way valve 1, the hydrochloric acid carrier liquid of input flows to the six-way valve in, be equipped with sample solution passageway 2 on the introduction port of six-way valve 1, namely sample solution directly pours into six-way valve 1 into from sample solution passageway 2 and mixes with the hydrochloric acid carrier liquid in six-way valve 1, be equipped with mixed liquid outlet pipe 6 on the appearance outlet of six-way valve 1, mixed liquid outlet pipe 6 is linked together with reaction liquid passageway 5, the mixed liquid (hydrochloric acid carrier liquid and sample solution) in six-way valve 1 mixes with the sodium borohydride reaction liquid in the reaction liquid passageway 5 through mixed liquid outlet pipe 6, the other end of the mixed liquid eduction tube 6 is connected with a tubular reactor 7 (the tubular reactor 7 is designed into a spiral shape), a microwave heater 17 is arranged on the tubular reactor 7, the liquid outlet of the tubular reactor 7 is connected with the liquid inlet 8 of the gas-liquid separator 9, the gas inlet of the gas-liquid separator 9 is connected with a carrier gas pipeline 11, the carrier gas pipeline 11 is used for inputting carrier gas (discharge gas), the gas and the input carrier gas are mixed after the reaction liquid reacted in the tubular reactor 7 enters the gas-liquid separator 9 and flows out along with the carrier gas from the gas outlet 12 above, the lower end of the mixed liquid eduction tube is provided with a waste liquid outlet 10 used for discharging the liquid of the reaction liquid, the gas outlet 12 above the gas-liquid separator 9 is connected with a drier 13 through a pipeline, and the gas outlet of the drier.
The utility model discloses a theory of operation does:
starting a multi-channel peristaltic pump 3, inputting hydrochloric acid carrier liquid into a six-way valve 1 through a carrier liquid channel 4, inputting sodium borohydride reaction liquid into a reaction liquid channel 5, conveying a sample solution from a sample solution channel 2 to the six-way valve 1, mixing the sample solution with the hydrochloric acid carrier liquid in the six-way valve 1, and then flowing out of the six-way valve 1 through a mixed liquid leading-out tube 6 and mixing the mixed solution with the sodium borohydride reaction liquid in the reaction liquid channel 5; the mixed solution enters a tubular reactor 7, and is heated by a microwave heater 17, tin is oxidized into tetravalent tin under the action of hydrochloric acid heating digestion, and tin hydride is generated under the action of sodium borohydride; after the reaction liquid enters the gas-liquid separator 9, gas-liquid separation is carried out, carrier gas is input into the gas-liquid separator 9 through a carrier gas pipeline 11, the separated gas flows out from a gas outlet 12 at the upper end of the gas-liquid separator 9 along with the carrier gas, and the liquid of the reaction liquid flows out from a waste liquid port 10 at the lower end of the gas-liquid separator 9; the gas flowing out of the gas-liquid separator 9 is further dried by a dryer 13 and then enters a glow discharge device 15, a spectrum signal emitted by tin atoms is generated under the excitation action of micro-plasmas in the glow discharge device 15, the residual waste gas flows out of a waste gas port 14 of the glow discharge device 15, then a CCD spectrometer 16 is used for collecting the spectrum signal emitted by the tin atoms, the intensity of the emitted spectrum signal is in direct proportion to the concentration of tin in a sample solution, the spectrum signal emitted by the tin atom in the standard solution is collected, the spectrum signal emitted by the tin atom in the sample solution to be detected is compared, and the quantitative detection of the tin content in the sample to be detected is realized according to the change of the signal intensity.
Although the present invention has been described with reference to the above preferred embodiments, it is not intended to limit the scope of the present invention, and those skilled in the art can make various changes and modifications with respect to the above preferred embodiments without departing from the spirit and scope of the present invention.
The protection scope of the present invention should be subject to the claims.

Claims (3)

1. The utility model provides a miniaturized detection device of tin content based on atomic emission spectroscopy which characterized in that: including multichannel peristaltic pump and six-way valve, set up carrier liquid passageway and reaction liquid passageway on the multichannel peristaltic pump, wherein, the carrier liquid passageway is connected with the inlet of six-way valve, be equipped with the sample solution passageway on the introduction port of six-way valve, be equipped with mixed liquid outlet pipe on the appearance mouth of six-way valve, mixed liquid outlet pipe is linked together with the reaction liquid passageway, the other end and the tubular reactor of mixed liquid outlet pipe are connected, set up the heater on the tubular reactor, tubular reactor's liquid outlet passes through the pipeline and is connected with vapour and liquid separator's inlet, vapour and liquid separator's air inlet and carrier gas pipeline are connected, vapour and liquid separator's gas outlet passes through the pipeline and is connected with the air inlet of desicator, the gas outlet of.
2. The miniaturized detection device of tin content based on atomic emission spectroscopy of claim 1, wherein: the tubular reactor is designed as a helical tubular reactor.
3. The miniaturized detection device of tin content based on atomic emission spectroscopy of claim 1, wherein: the heater is a microwave heater or an electric heater.
CN202020191949.5U 2020-02-21 2020-02-21 Miniaturized detection device of tin content based on atomic emission spectroscopy Expired - Fee Related CN212341012U (en)

Priority Applications (1)

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CN202020191949.5U CN212341012U (en) 2020-02-21 2020-02-21 Miniaturized detection device of tin content based on atomic emission spectroscopy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202020191949.5U CN212341012U (en) 2020-02-21 2020-02-21 Miniaturized detection device of tin content based on atomic emission spectroscopy

Publications (1)

Publication Number Publication Date
CN212341012U true CN212341012U (en) 2021-01-12

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Granted publication date: 20210112