CN104990910A - Pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and analysis method - Google Patents
Pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and analysis method Download PDFInfo
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Abstract
The invention provides a pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and an analysis method, and the pre-concentration tandem arrangement comprises a tungsten pre-concentration device, an electrothermal vaporization device, a torch interface, a carrier gas mass flowmeter, an auxiliary gas mass flowmeter, a diverter three-way, a converging three-way, a carrier gas channel, an auxiliary gas channel and the like. An inductively coupled plasma emission spectrometry for measuring solid sampling of the zinc comprises the steps of dehydrating and ashing a sample to be measured in air to obtain inorganic residues; heating the sample residues at about 1600 DEG C under an argon hydrogen mixture atmosphere, the evaporated aerosol containing zinc atoms contacts with tungsten filament, and the zinc is pre-concentrated by the tungsten filament; heating the temperature of the tungsten filament to be about 1800 DEG C, releasing the zinc atoms, and analyzing the content of the zinc by the inductive coupling plasma emission spectrograph. The pre-concentration tandem arrangement has a simple structure and the problems that a plasma torch is extinguished and a signal is unstable when the tungsten pre-concentration device and the electrothermal vaporization device are in combination with the inductively coupled plasma emission spectrometry are solved. The pre-concentration tandem arrangement has the advantages that the digestion treatment is not needed to be performed on the sample, the trace zinc in the sample can be measured, and the pre-concentration tandem arrangement has the characteristics such as being direct, speediness, high sensitivity and good stability.
Description
Technical field
The present invention relates to chemical analysis detection field, be specifically related to preenrichment tandem arrangement and analytical approach that a kind of solid sampling inductively coupled plasma emission spectrography surveys 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/T 5009.14-2003 " mensuration of Zinc in Foods ", GB 5413.21-2010 " calcium in national food safety standard infant food and dairy products, iron, zinc, sodium, potassium, magnesium, the mensuration of copper and manganese ", GB/T 9695.20-2008 " meat quail. Direct spectrophotometry ", GB/T 23375-2009 " copper in vegetables and goods thereof, iron, zinc, calcium, magnesium, phosphorus yield ", GB/T 17138-1997 " 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, ETV-ICP-AES is because its antijamming capability is comparatively strong, linear dynamic range is wide and the ability of Simultaneous multi element analysis, enjoys researcher to pay close attention in solid sampling spectral technique.
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 in inductance coupling plasma emissioning spectral analysis.
Summary of the invention
The object of the invention is for the problems referred to above, a kind of solid sampling inductively coupled plasma emission spectrography is provided to survey the preenrichment tandem arrangement of zinc, this apparatus structure is simple, when solving tungsten filament preenrichment device and electric heating evaporation device and inductive coupling plasma emission spectrograph coupling, plasma puts out a difficult problem for torch, jitter, without the need to clearing up process to sample, the detection to wherein trace zinc can be realized, there is the features such as direct, quick, highly sensitive, good stability.
Survey zinc solid sampling inductive coupling plasma emission spectrograph coupling arrangement provided by the present invention, be made up of tungsten filament preenrichment device 10, electric heating evaporation device 7, torch interface tube 13, interflow threeway 11, carrier gas mass flowmeter 4, assisted gas mass flowmeter 6, diversion three-way 2, carrier gas gas circuit 3, assisted gas gas circuit 5, wherein said tungsten filament preenrichment device 10 is made up of tungsten filament 8, power socket 9 and preenrichment device 10 cavity.Described carrier gas gas circuit 3 is connected with argon hydrogen combination gas source of the gas 1 by diversion three-way 2 with the right-hand member gas access of assisted gas gas circuit 5, described carrier gas gas circuit 3 connects diversion three-way 2, carrier gas mass flowmeter 4, electric heating evaporation device 7, tungsten filament preenrichment device 10, interflow threeway 11 successively, and described assisted gas gas circuit 5 connects diversion three-way 2, assisted gas mass flowmeter 6, interflow threeway 11 successively; The right-hand member of described torch interface tube 13 is connected with interflow threeway 11 by interflow gas circuit 12, and left end is connected with inductive coupling plasma emission spectrograph 14.
Further, preferred version is: described argon hydrogen combination gas is the argon hydrogen combination gas containing 2%-4% (volume ratio) hydrogen.
Further, preferred version is: described boat shape injector 15, electric evaporator 7 are foamed carbon material.
Further, preferred version is: described tungsten filament preenrichment device 10 cavity is aluminum material.
Further, preferred version is: described carrier gas gas circuit 3, assisted gas gas circuit 5, interflow gas circuit 12, torch interface tube 13 are teflon material.
The inductively coupled plasma atomic emission combination analysis method of mensuration zinc provided by the present invention, comprises the steps:
A: about 500 DEG C in atmosphere, by the food samples dehydration to be measured in boat shape injector 15, ashing, remove most of organic substance;
B: described carrier gas gas circuit 3 is by carrier gas mass flowmeter 4, accurately the argon hydrogen combination gas containing 2%-4% (volume ratio) hydrogen of certain flow rate is passed into electric evaporator 7, ash residue is warming up to about 1600 DEG C by electric evaporator 7, what evaporation obtained contacts with the tungsten filament 8 in tungsten filament preenrichment device 10 containing zinc gasoloid, and wherein zinc is caught by tungsten filament 8;
C: under the argon hydrogen combination gas atmosphere containing 2%-4% (volume ratio) hydrogen, tungsten filament 8 temperature is elevated to about 1800 DEG C by power socket 9, the zinc discharged enters interflow threeway 11 with argon hydrogen combination gas;
D: the argon hydrogen combination gas containing 2%-4% (volume ratio) hydrogen is passed into assisted gas mass flowmeter 6 by assisted gas gas circuit 5, collaborate at interflow threeway 11 and tungsten filament preenrichment device 10 zinc out, enter torch interface tube 13 by interflow gas circuit 12, then enter the content that inductive coupling plasma emission spectrograph 14 analyzes zinc.
Remarkable advantage of the present invention is:
1, a bottleneck difficult problem for tungsten filament preenrichment device and electric heating evaporation device and inductive coupling plasma emission spectrograph coupling is solved---stable plasma torch flame, overcomes the airflow fluctuation caused because tungsten filament preenrichment device and electric heating evaporation device connect and the plasma torch flame of inductive coupling plasma emission spectrograph is stopped working problem.
2, there is two gas circuit pattern: by two mass-flow gas meter, achieve the air-flow precise hard_drawn tuhes of carrier gas gas circuit and assisted gas gas circuit, improve the stability of plasma torch flame.
Accompanying drawing illustrates:
Below with reference to accompanying drawing and instantiation, the present invention will be further elaborated.
Fig. 1-solid sampling inductively coupled plasma emission spectrography surveys the preenrichment tandem arrangement of zinc;
Wherein 1-argon hydrogen combination gas source of the gas, 2-diversion three-way, 3-carrier gas gas circuit, 4-carrier gas mass flowmeter, 5-assisted gas gas circuit, 6-assisted gas mass flowmeter, 7-electric evaporator, 8-tungsten filament, 9-power socket, 10-tungsten filament preenrichment device, 11-collaborates threeway, and 12-collaborates gas circuit, 13-torch interface tube, 14-inductive coupling plasma emission spectrograph, 15-boat shape injector.
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
Before the solid sample feeding device sample introduction that the standard solution containing cadmium is formed at tungsten filament preenrichment device 10 and electric evaporator 7, the dividing potential drop of the argon hydrogen combination gas source of the gas 1 containing 2% hydrogen is set in about 0.5Mpa, carrier gas mass flowmeter 4 is set as 800mL/min, assisted gas mass flowmeter 6 is set as 300mL/min, zinc is evaporated in electric evaporator 7, and caught by tungsten filament preenrichment device 10 and discharge again, gasoloid containing atomic state zinc enters interflow threeway 11 in carrier gas gas circuit 3, collaborating to mix in threeway 11 with the argon hydrogen combination gas flowed out in assisted gas mass flowmeter 6 again, the mixed zinc gasoloid that contains enters torch interface tube 13 by interflow gas circuit 12, enter inductive coupling plasma emission spectrograph 14 again.Under solid sample feeding device 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 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 4% hydrogen as source of the gas, carrier gas mass flowmeter 4 is set as 700mL/min, connect with inductive coupling plasma emission spectrograph with tungsten filament preenrichment device of the present invention and electric evaporator, other conditions are identical with embodiment one.In 3 working samples, the content of zinc is 14.9 ± 1.1 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 6.1%.
Embodiment three
For 2mg soil powder (GB thing GBW07401), use the argon hydrogen combination gas containing 4% hydrogen as source of the gas, carrier gas mass flowmeter 4 is set as 700mL/min, connect with inductive coupling plasma emission spectrograph with tungsten filament preenrichment device of the present invention and electric evaporator, other conditions are identical with embodiment one.In 3 working samples, the content of zinc is 694.5 ± 53.2 mg/kg, and within standard value 680 ± 25 mg/kg of this standard substance, the relative standard deviation measuring 7 times is 7.3%.
Above-mentioned three examples illustrate a kind of tungsten filament preenrichment devices provided by the invention and electric evaporator and inductive coupling plasma emission spectrograph coupling arrangement, can ensure the stability of inductively coupled plasma emission spectrography survey zinc, sensitivity and accuracy.
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 (10)
1. the preenrichment tandem arrangement of an emission spectrometry survey zinc, be made up of tungsten filament preenrichment device, electric heating evaporation device, torch interface tube, interflow threeway, carrier gas mass flowmeter, assisted gas mass flowmeter, diversion three-way, carrier gas gas circuit, assisted gas gas circuit, wherein said tungsten filament preenrichment device is made up of tungsten filament, power socket and preenrichment device cavity.
2. the tungsten filament preenrichment device measuring zinc as claimed in claim 1, is characterized in that: described carrier gas gas circuit is connected with argon hydrogen combination gas source of the gas by diversion three-way with the right-hand member gas access of assisted gas gas circuit.
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 diversion three-way, carrier gas mass flowmeter, electric heating evaporation device, tungsten filament preenrichment device, interflow threeway successively.
4. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described assisted gas gas circuit connects diversion three-way, assisted gas mass flowmeter, interflow threeway successively.
5. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: the right-hand member of described torch interface tube is connected with interflow threeway by interflow gas circuit, and left end is connected with inductive coupling plasma emission spectrograph.
6. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described argon hydrogen combination gas is the argon hydrogen combination gas containing 2%-4% hydrogen.
7. 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.
8. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described tungsten filament preenrichment device cavity is aluminum material.
9. the tungsten filament preenrichment device measuring zinc as claimed in claim 1 or 2, is characterized in that: described carrier gas gas circuit, assisted gas gas circuit, interflow gas circuit, torch interface tube are teflon material.
10. adopt the assay method of the tungsten filament preenrichment device of the mensuration zinc as described in one of claim 1-9, it is characterized in that: comprise the steps:
A: about 500 DEG C in atmosphere, by the food samples dehydration to be measured in boat shape injector, ashing, remove most of organic substance;
B: described carrier gas gas circuit is by carrier gas mass flowmeter, accurately the argon hydrogen combination gas containing 2%-4% hydrogen of certain flow rate is passed into electric evaporator, ash residue is warming up to about 1600 DEG C by electric evaporator, evaporate the tungsten wire contact contained in zinc gasoloid and tungsten filament preenrichment device obtained, wherein zinc is caught by tungsten filament;
C: under the argon hydrogen combination gas atmosphere containing 2%-4% hydrogen, tungsten filament temperature is elevated to about 1800 DEG C by power socket, and the zinc discharged enters interflow threeway with argon hydrogen combination gas;
D: the argon hydrogen combination gas containing 2%-4% hydrogen is passed into assisted gas mass flowmeter by assisted gas gas circuit, collaborate in interflow threeway and tungsten filament preenrichment device zinc out, enter torch interface tube by interflow gas circuit, then enter the content that inductive coupling plasma emission spectrograph analyzes zinc.
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Cited By (2)
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| CN105606692A (en) * | 2016-03-11 | 2016-05-25 | 中国农业科学院农业质量标准与检测技术研究所 | Device for detecting zinc through inductively coupled plasma mass spectrometry method and analysis method |
| CN110470527A (en) * | 2018-05-11 | 2019-11-19 | 中国石油化工股份有限公司 | A kind of dry gas quantifies enrichment system and method |
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Cited By (3)
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| CN105606692A (en) * | 2016-03-11 | 2016-05-25 | 中国农业科学院农业质量标准与检测技术研究所 | Device for detecting zinc through inductively coupled plasma mass spectrometry method and analysis method |
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| CN110470527B (en) * | 2018-05-11 | 2022-07-15 | 中国石油化工股份有限公司 | Dry gas quantitative enrichment system and method |
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