CN204789103U - A tungsten filament pre -concentration device for determining zinc - Google Patents
A tungsten filament pre -concentration device for determining zinc Download PDFInfo
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- CN204789103U CN204789103U CN201520504183.0U CN201520504183U CN204789103U CN 204789103 U CN204789103 U CN 204789103U CN 201520504183 U CN201520504183 U CN 201520504183U CN 204789103 U CN204789103 U CN 204789103U
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- preenrichment
- atomic fluorescence
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Abstract
The utility model provides a tungsten filament pre -concentration device for determining zinc, the device is including boat form injector, electric heat evaporation plant, pre -concentration device, carrier gas gas circuit, carrier gas mass flow meter, release gas circuit, atomic fluorescence spectrum appearance etc. The solid of survey zinc advances a kind atomic fluorescence spectrometry, with need checking sample dehydration, ashing, obtains the inorganic matter residue in the air, under argon hydrogen gas mixture atmosphere, will the sample residue heaies up to 1600 DEG C of left and right sides, contains the aerosol and tungsten filament contact of zinc atom, and zinc is by the tungsten filament pre -concentration, the tungsten filament temperature rises to 1800 DEG C of left and right sides, releases the zinc atom, the content of atomic fluorescence spectrum appearance analysis zinc. The device has solved the solid and has advanced the matrix interference difficult problem that kind electric heat evaporation atomic fluorescence spectrometry surveyed zinc, and its advantage lies in need not clearing up the processing to the sample, can realize wherein accuracy, the stability analysis of zinc content.
Description
Technical field
The utility model relates to chemical analysis detection field, is specifically related to a kind of tungsten filament preenrichment device for measuring zinc.
Technical background
Zinc is human essential elements, is the index of conventional sense in the field such as food, health; Meanwhile, excessive zinc also can work the mischief to human body, and particularly the utilising zinc containing waste residue of industrial and mining enterprises, discharge of wastewater can destroy ecologic environment, and affect health by biologic chain.At present, measure the instrument of Zinc in Foods and method with Liquid sample introduction system for mainstream technology, the country of current element analysis and the industry standard overwhelming majority are the atomic absorption spectrography (AAS)s (AAS) adopting Liquid sample introduction, atomic fluorescence spectrometry (AFS), inductively coupled plasma emission spectrography (ICP-AES), the methods such as inductively coupled plasma mass spectrometry (ICP-MS), such as GB/T5009.14-2003 " mensuration of Zinc in Foods ", GB5413.21-2010 " calcium in national food safety standard infant food and dairy products, iron, zinc, sodium, potassium, magnesium, the mensuration of copper and manganese ", GB/T9695.20-2008 " meat quail. Direct spectrophotometry ", GB/T23375-2009 " copper in vegetables and goods thereof, iron, zinc, calcium, magnesium, phosphorus yield ", GB/T17138-1997 " soil quality copper, Direct spectrophotometry atomic absorption spectrophotometry " etc.Liquid sample introduction needs to carry out Specimen eliminating process in advance, by ashing and the process such as strong acid and strong oxidizer, complicated organic sample is converted to simple inorganic matrix, thus reduces Matrix effects and the loss to instrument.Liquid sample introduction system is easy to robotization, but sample introduction efficiency is lower, as atomizer sample introduction efficiency only have 10% ~ 15%, simultaneously sample pretreatment process that is complicated, consuming time, that require great effort greatly limit spectrographic technique at the scene, the application in express-analysis field.
Solid sampling method was just applied in the atomic spectrum early stage of development, and such as NaCl is directly imported the research of graphite furnace atomizer by nineteen fifty-seven L ' vov.But be limited to the rapid rising of technical conditions at that time and Liquid sample introduction system, solid sampling method does not obtain enough attention and development as the branch of spectral analysis technique.In recent years, along with material science, electric heating evaporation (ETV), laser ablation (LA), atom trap such as to catch at the high-level efficiency Sample introduction technology, background correction and the multielement sequential analytical technologies such as Zeeman effect, charge-coupled image sensor (CCD) and continuous light source (CS), and the development and application of the technology such as matrix modifier and Spectroscopy With Suspension-injection is promoted, the analysis means of solid sampling and obtaining the analysis ability of sample significantly promotes.Wherein, atomic fluorescence spectrometer is the large-scale spectrometric instrument that China's minority has independent intellectual property right, and the development of solid sampling atomic fluorescence spectrometer can promote the scene of atomic fluorescence device in Element detection, rapid, miniaturization further.
Although the spectral instrument of Direct solid sampling can adopt certain background correction technology to alleviate Matrix effects impact, but this is a kind of remedial technique, and the complicated substrate that solid sampling process is brought and spectra1 interfer-are restriction ETV solid sampling development and application bottleneck problem always.It is a kind of very effective solid sampling Matrix effects technology for eliminating that atom trap is caught, such as, utilize the survey mercury solid sample feeding device of gold amalgam principle, utilize tungsten filament to catch the survey cadmium solid sample feeding device of cadmium principle.Above-mentioned technology utilizes spun gold/tungsten filament can catch atomic state mercury/cadmium at normal temperatures, and at high temperature can effectively discharge mercury/cadmium, then can realize preenrichment and Matrix separation two targets, thus effectively alleviate Matrix effects by catching of mercury/cadmium with Matrix separation.At present, there is not yet and utilize tungsten filament preenrichment zinc to eliminate the report of Matrix effects.
Summary of the invention
The purpose of this utility model is for the problems referred to above, a kind of tungsten filament preenrichment device for solid sampling Electrothermal evaporation atomic fluorescence spectrographic determination zinc is provided, this apparatus structure is simple, solve the Matrix effects difficult problem that solid sampling Electrothermal evaporation atomic fluorescence spectroscopic methodology surveys zinc, without the need to clearing up process to sample, accurate, the stability analysis of wherein Zn content can be realized.
The tungsten filament preenrichment device of solid sampling Electrothermal evaporation atomic fluorescence spectrographic determination zinc provided by the utility model, by comprising boat shape injector, electric heating evaporation device, preenrichment device, carrier gas gas circuit, carrier gas mass flowmeter, release gas circuit, atomic fluorescence spectrometer, described preenrichment device is made up of tungsten filament, tungsten filament power socket and preenrichment device cavity, described tungsten filament is arranged on tungsten filament power socket, makes somebody a mere figurehead and is placed in preenrichment device cavity central authorities; Described electric heating evaporation device is made up of electric evaporator, electric heating evaporation device cavity, electric evaporator power supply; Described carrier gas gas circuit connects argon hydrogen combination gas source of the gas, mass flowmeter, electric heating evaporation device and preenrichment device successively, and described release gas circuit connects grabber cavity outlet and atomic fluorescence spectrometer.
Further, described scheme is preferably: described argon hydrogen combination gas is the argon hydrogen combination gas containing 10%-80% (volume ratio) hydrogen.
Further, described scheme is preferably: described boat shape injector 12, electric evaporator 6 are foamed carbon material.
Further, described scheme is preferably: described electric heating evaporation device 4 cavity, preenrichment device 7 cavity are aluminum material.
Further, described scheme is preferably: described carrier gas gas circuit 3 is silica gel hose material, and described release gas circuit 10 is teflon hose material.
The solid sampling atomic fluorescence spectrophotometry combination analysis method of mensuration zinc provided by the utility model, comprises the steps:
About 500 DEG C in atmosphere, by the testing sample dehydration in boat shape injector 12, ashing, remove most of organic substance;
The argon hydrogen combination gas containing 10%-80% (volume ratio) hydrogen of certain flow rate, by carrier gas mass flowmeter 2, is accurately passed into electric heating evaporation device 4 by described carrier gas gas circuit 3;
Boat shape injector 12 is sent in electric evaporator 6 by sample introduction arm 13, and sample ashing residue is warming up to about 1600 DEG C by electric evaporator 6, and what obtain contacts with the tungsten filament 8 of preenrichment device 7 containing zinc gasoloid, and wherein zinc is caught by tungsten filament 8;
Under argon hydrogen combination gas atmosphere, tungsten filament temperature is elevated to about 1800 DEG C by tungsten filament power socket 9, and the zinc discharged enters release gas circuit 10 with argon hydrogen combination gas, then enters the content that atomic fluorescence spectrometer 11 analyzes zinc.
The beneficial effect of the invention:
Remarkable advantage of the present utility model is: apparatus structure is simple, handled easily; Solve the Matrix effects difficult problem that solid sampling Electrothermal evaporation atomic fluorescence spectroscopic methodology surveys zinc, without the need to clearing up process to sample; The detection system built can realize accurate, the stability analysis of wherein Zn content, reproducible, error is little.
Accompanying drawing illustrates:
Below with reference to accompanying drawing and instantiation, the present invention will be further elaborated.
Fig. 1-for the tungsten filament preenrichment device of solid sampling Electrothermal evaporation atomic fluorescence spectrographic determination zinc;
Wherein 1-argon hydrogen combination gas source of the gas, 2-carrier gas mass flowmeter, 3-carrier gas gas circuit, 4-electric heating evaporation device, 5-electric evaporator power supply, 6-electric evaporator, 7-preenrichment device, 8-tungsten filament, 9-tungsten filament power socket, 10-discharges gas circuit, 11-atomic fluorescence spectrometer, 12-boat shape injector, 13-sample introduction arm.
Embodiment:
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Unless otherwise defined, all specialties used in literary composition and scientific words and one skilled in the art the meaning be familiar with identical.In addition, any method similar or impartial to described content and material all can be applicable in the present invention.The use that better implementation method described in literary composition and material only present a demonstration.
Embodiment one
When the standard solution containing zinc is before electric heating evaporation solid sample feeding device sample introduction caught by tungsten filament, the dividing potential drop of the argon hydrogen combination gas source of the gas 1 containing 10% hydrogen is set in about 0.5Mpa, carrier gas mass flowmeter 2 is set as 600mL/min, zinc is evaporated in electric heating evaporation device 4, and caught by tungsten filament 8 and discharge again, the gasoloid containing atomic state zinc enters atomic fluorescence spectrometer 11 by release gas circuit 10.In optimal conditions, the range of linearity surveying zinc is 0 ~ 2.5 μ g, and the regression coefficient of typical curve is more than 0.995, and the detection limit of zinc can reach 0.1pg, and the relative standard deviation repeatedly measured is within 5%.
Embodiment two
For 5mg ground rice (GB thing GBW10045), use the argon hydrogen combination gas containing 10% hydrogen as source of the gas, carrier gas mass flowmeter 2 is set as 700mL/min, coordinate electric heating evaporation solid sample feeding device to connect with atomic fluorescence spectrometer with zinc preenrichment device of the present invention, other conditions are identical with embodiment one.In working sample, zinc is 13.9 ± 0.3 mg/kg, and within standard value 14.4 ± 0.8 mg/kg of this standard substance, the relative standard deviation measured for 7 times is 7.1%.
Embodiment three
For 2mg soil powder (GB thing GBW07401), use the argon hydrogen combination gas containing 10% hydrogen as source of the gas, carrier gas mass flowmeter 2 is set as 700mL/min, coordinate electric heating evaporation solid sample feeding device to connect with atomic fluorescence spectrometer with zinc preenrichment device of the present invention, other conditions are identical with embodiment one.In working sample, zinc is 703.5 ± 33.2 mg/kg, and within standard value 680 ± 25 mg/kg of this standard substance, the relative standard deviation measuring 7 times is 8.3%.
Above-mentioned three examples illustrate a kind of tungsten filament preenrichment device for solid sampling Electrothermal evaporation atomic fluorescence spectrographic determination zinc provided by the invention and using method, effectively can eliminate Matrix effects when surveying zinc, can ensure the Stability and veracity of mensuration.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (6)
1. one kind for measuring the tungsten filament preenrichment device of zinc, its composition comprises boat shape injector, electric heating evaporation device, preenrichment device, carrier gas gas circuit, carrier gas mass flowmeter, release gas circuit, atomic fluorescence spectrometer, it is characterized in that: described preenrichment device is made up of tungsten filament, tungsten filament power socket and preenrichment device cavity, described tungsten filament is arranged on tungsten filament power socket, makes somebody a mere figurehead and is placed in preenrichment device cavity central authorities.
2. the tungsten filament preenrichment device measuring zinc as claimed in claim 1, is characterized in that: described electric heating evaporation device is made up of electric evaporator, electric heating evaporation device cavity, electric evaporator power supply.
3. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described carrier gas gas circuit connects argon hydrogen combination gas source of the gas, mass flowmeter, electric heating evaporation device and preenrichment device successively.
4. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described boat shape injector, electric evaporator are foamed carbon material.
5. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described electric heating evaporation device cavity, preenrichment device cavity are aluminum material.
6. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, it is characterized in that: described carrier gas gas circuit is silica gel hose material, described release gas circuit is teflon hose material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520504183.0U CN204789103U (en) | 2015-07-13 | 2015-07-13 | A tungsten filament pre -concentration device for determining zinc |
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| CN201520504183.0U CN204789103U (en) | 2015-07-13 | 2015-07-13 | A tungsten filament pre -concentration device for determining zinc |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104990785A (en) * | 2015-07-13 | 2015-10-21 | 中国农业科学院农业质量标准与检测技术研究所 | Tungsten filament pre-enrichment device for determining zinc and using method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104990785A (en) * | 2015-07-13 | 2015-10-21 | 中国农业科学院农业质量标准与检测技术研究所 | Tungsten filament pre-enrichment device for determining zinc and using method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: YUNNAN CTI CERTIFICATION CO.,LTD. Assignor: INSTITUTE OF QUALITY STANDARD AND TESTING TECHNOLOGY FOR AGRO-PRODUCTS, CHINESE ACADAMY OF AGRICULTURAL SCIENCES Contract record no.: X2022990000945 Denomination of utility model: A tungsten wire preconcentration device for zinc determination Granted publication date: 20151118 License type: Common License Record date: 20221115 |
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| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Beijing Jitian Instrument Co.,Ltd. Assignor: INSTITUTE OF QUALITY STANDARD AND TESTING TECHNOLOGY FOR AGRO-PRODUCTS, CHINESE ACADAMY OF AGRICULTURAL SCIENCES Contract record no.: X2023980033481 Denomination of utility model: A Tungsten Wire Preconcentration Device for the Determination of Zinc Granted publication date: 20151118 License type: Common License Record date: 20230309 |
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| EE01 | Entry into force of recordation of patent licensing contract |