CN104990910B - A kind of emission spectrometry surveys the preenrichment tandem arrangement and analysis method of zinc - Google Patents
A kind of emission spectrometry surveys the preenrichment tandem arrangement and analysis method of zinc Download PDFInfo
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- CN104990910B CN104990910B CN201510409052.9A CN201510409052A CN104990910B CN 104990910 B CN104990910 B CN 104990910B CN 201510409052 A CN201510409052 A CN 201510409052A CN 104990910 B CN104990910 B CN 104990910B
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Abstract
The present invention provides preenrichment tandem arrangements and analysis method that a kind of emission spectrometry surveys zinc, including tungsten wire preenrichment device, electric heating evaporation device, torch pipe interface, carrier gas mass flowmenter, auxiliary gas mass flowmenter, diversion three-way, interflow threeway, carrier gas gas circuit, auxiliary gas gas circuit etc..The solid sampling inductively coupled plasma emission spectrography of zinc is measured, including sample to be tested dehydration, ashing are obtained into mineral residue in air；Under argon hydrogen gaseous mixture atmosphere, the sample residue is warming up to 1600 DEG C or so, the aerosol and tungsten wire contact containing zinc atom evaporated, zinc is by tungsten wire preenrichment；The tungsten wire temperature rises to 1800 DEG C or so, releases zinc atom, and inductive coupling plasma emission spectrograph analyzes the content of zinc.The apparatus structure is simple, solves the problems, such as that plasma puts out torch, jitter when tungsten wire preenrichment device and electric heating evaporation device and inductive coupling plasma emission spectrograph are combined.The advantage of the invention is that the detection to wherein trace zinc can be realized without carrying out resolution processing to sample, have the characteristics that direct, quick, high sensitivity, stability are good.
Description
Technical field
The present invention relates to chemical analysis and testing areas, and in particular to a kind of solid sampling inductively coupled plasma body transmitting light
The preenrichment tandem arrangement and analysis method of spectrometry survey zinc.
Technical background
Zinc is human essential elements, is the index of conventional detection in fields such as food, health；Meanwhile excessive zinc also can
It does harm to huamn body, the utilising zinc containing waste residue, discharge of wastewater of especially industrial and mining enterprises can destroy ecological environment, and pass through biological chain shadow
Ring human health.Currently, the instrument and method of measurement Zinc in Foods are using Liquid sample introduction system as mainstream technology, current element is analyzed
Country and the professional standard overwhelming majority be all using the atomic absorption spectrography (AAS) (AAS) of Liquid sample introduction, atomic fluorescence spectrometry
(AFS), inductively coupled plasma
The methods of body emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), such as GB/T
5009.14-2003 " measurement of Zinc in Foods ", GB 5413.21-2010 " national food safety standard infant food and dairy products
The measurement of middle calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese ", GB/T 9695.20-2008 " meat and meat products Direct spectrophotometry ", GB/T
23375-2009 " copper, iron, zinc, calcium, magnesium, phosphorus yield in vegetables and its product ", GB/T 17138-1997 " soil quality copper,
Direct spectrophotometry atomic absorption spectrophotometry " etc..Liquid sample introduction needs to carry out Specimen eliminating processing in advance, by be ashed with
And complicated organic sample is converted to simple inorganic matrix by the processing such as strong acid and strong oxidizer, to reduce Matrix effects and right
The loss of instrument.Liquid sample introduction system is easy to automate, but sample introduction efficiency is lower, and such as general atomizer sample introduction efficiency only has
10%~15%, while complicated, time-consuming, laborious sample pretreatment process greatly limits spectrographic technique and at the scene, quickly divides
The application in analysis field.
Solid sampling method has just been applied in the atom spectrum early stage of development, such as nineteen fifty-seven L ' vov NaCl is straight
Connect the research for importing graphite furnace atomizer.But it is limited to the quick emerging of technical conditions at that time and Liquid sample introduction system
It rises, solid sampling method does not obtain enough attention and development as the branch of spectral analysis technique.In recent years, with material
Material science, the high efficiency Sample introduction technologies such as electric heating evaporation (ETV), laser ablation (LA), atom trap capture, Zeemen effect, electricity
The background corrections such as lotus coupled apparatus (CCD) and continuous light source (CS) and multielement sequential analytical technology and matrix modifier and
The development and application of the technologies such as Spectroscopy With Suspension-injection, the analysis means of solid sampling and have obtained greatly the analysis ability of sample
Amplitude is promoted.Wherein, ETV-ICP-AES is because its anti-interference ability is wide compared with strong, linear dynamic range and Simultaneous multi element analysis
Ability is paid close attention in solid sampling spectral technique by researcher.
Although the spectral instrument of Direct solid sampling can mitigate Matrix effects shadow using certain background correction technology
It rings, but this is a kind of remedial technique, and complicated substrate brought by solid sampling process and spectra1 interfer- are always to limit ETV
Solid sampling develops and applies bottleneck problem.Atom trap capture is a kind of very effective solid sampling Matrix effects elimination skill
Art, such as catch using the survey mercury solid sample feeding device of gold amalgam principle, using tungsten wire the survey cadmium solid sample feeding device of cadmium principle.On
Atomic state mercury/cadmium can be captured using spun gold/tungsten wire at normal temperature by stating technology, and can be released effectively mercury/cadmium at high temperature, be passed through
Preenrichment then may be implemented for the capture of mercury/cadmium and matrix separation and matrix separates two targets, to effectively mitigate Matrix effects.
Currently, there is not yet using tungsten wire preenrichment zinc to eliminate Matrix effects in terms of inductance coupling plasma emissioning spectral analysis
Report.
Summary of the invention
Regarding the issue above, the present invention provides a kind of solid sampling inductively coupled plasma emission spectrography
The preenrichment tandem arrangement of zinc is surveyed, the apparatus structure is simple, solves tungsten wire preenrichment device and electric heating evaporation device and inductance
Plasma puts out the problem of torch, jitter when coupled plasma optical emission spectrometer is combined, without clearing up to sample
Processing, can be realized the detection to wherein trace zinc, have the characteristics that direct, quick, high sensitivity, stability are good.
Survey zinc solid sampling inductive coupling plasma emission spectrograph coupling arrangement provided by the present invention, it is pre- by tungsten wire
Enriching apparatus 10, electric heating evaporation device 7, torch pipe interface 13, interflow threeway 11, carrier gas mass flowmenter 4, auxiliary gas mass flow
Meter 6, diversion three-way 2, carrier gas gas circuit 3, auxiliary gas gas circuit 5 form, wherein the tungsten wire preenrichment device 10 is by tungsten wire 8, power supply
Seat 9 and 10 cavity of preenrichment device composition.The right end gas access of the carrier gas gas circuit 3 and auxiliary gas gas circuit 5 is by diversion three-way 2
It is connect with argon hydrogen gaseous mixture gas source 1, the carrier gas gas circuit 3 is sequentially connected diversion three-way 2, carrier gas mass flowmenter 4, electric heating evaporation
Device 7, tungsten wire preenrichment device 10, interflow threeway 11, the auxiliary gas gas circuit 5 are sequentially connected diversion three-way 2, auxiliary makings amount
Flowmeter 6, interflow threeway 11；The right end of the torch pipe interface 13 by interflow gas circuit 12 with interflow threeway 11 connect, left end and
Inductive coupling plasma emission spectrograph 14 connects.
Further, preferred embodiment are as follows: the argon hydrogen gaseous mixture is the argon hydrogen containing 2% -4% (volume ratio) hydrogen
Gaseous mixture.
Further, preferred embodiment are as follows: the navicular sample injector 15, electric evaporator 7 are foamed carbon material.
Further, preferred embodiment are as follows: 10 cavity of tungsten wire preenrichment device is aluminum material.
Further, preferred embodiment are as follows: the carrier gas gas circuit 3, auxiliary gas gas circuit 5, interflow gas circuit 12, torch pipe interface 13
For polytetrafluoroethylene (PTFE) material.
The inductively coupled plasma atomic emission combination analysis method of measurement zinc provided by the present invention, including walk as follows
It is rapid:
A: 500 DEG C or so in air, by food samples to be measured dehydration, the ashing in navicular sample injector 15, remove big portion
Divide organic substance；
B: certain flow rate is accurately contained 2% -4% (body by carrier gas mass flowmenter 4 by the carrier gas gas circuit 3
Product ratio) the argon hydrogen gaseous mixture of hydrogen is passed through electric evaporator 7, and ash residue is warming up to 1600 DEG C or so by electric evaporator 7, is steamed
It sends out obtained aerosol containing zinc to contact with the tungsten wire 8 in tungsten wire preenrichment device 10, wherein zinc is captured by tungsten wire 8；C: containing
Under the argon hydrogen gaseous mixture atmosphere of 2% -4% (volume ratio) hydrogen, 8 temperature of tungsten wire is increased to 1800 DEG C or so by power socket 9, is released
The zinc of releasing enters interflow threeway 11 with argon hydrogen gaseous mixture；
D: the argon hydrogen gaseous mixture containing 2% -4% (volume ratio) hydrogen is passed through auxiliary gas mass flow by auxiliary gas gas circuit 5
Meter 6, collaborates in the zinc that interflow threeway 11 and tungsten wire preenrichment device 10 come out, and enters torch pipe interface 13 by interflow gas circuit 12,
Enter back into the content that inductive coupling plasma emission spectrograph 14 analyzes zinc.
Remarkable advantage of the invention is:
1, tungsten wire preenrichment device and electric heating evaporation device are solved and inductive coupling plasma emission spectrograph is combined
Bottleneck problem --- stable plasma torch flame, overcome due to tungsten wire preenrichment device and electric heating evaporation device connection and
Caused airflow fluctuation makes the flame-out problem of the plasma torch flame of inductive coupling plasma emission spectrograph.
2, there are double gas circuit modes: by double gas mass flow meters, realizing carrier gas gas circuit and assist the gas of gas gas circuit
The accurate control of stream, improves the stability of plasma torch flame.
Detailed description of the invention:
Below with reference to drawings and concrete examples, 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 gaseous mixture gas source, 2- diversion three-way, 3- carrier gas gas circuit, 4- carrier gas mass flowmenter, 5- assist gas
Gas circuit, 6- assist gas mass flowmenter, 7- electric evaporator, 8- tungsten wire, 9- power socket, 10- tungsten wire preenrichment device, 11- conjunction
Threeway is flowed, 12- collaborates gas circuit, 13- torch pipe interface, 14- inductive coupling plasma emission spectrograph, the navicular sample injector of 15-.
Specific embodiment:
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.Unless otherwise defined, all professional and scientific terms as used herein and this field
Meaning known to skilled person is identical.In addition, any method similar to or equal to what is recorded and material can all be applied
In the present invention.The preferred methods and materials described herein are for illustrative purposes only.
Embodiment one
When the solid sample feeding device that the standard solution containing zinc is constituted in tungsten wire preenrichment device 10 and electric evaporator 7 into
Before sample, the partial pressure of the argon hydrogen gaseous mixture gas source 1 containing 2% hydrogen is set in 0.5Mpa or so, carrier gas mass flowmenter 4 is set
For 800mL/min, gas mass flowmenter 6 is assisted to be set as 300mL/min, zinc is evaporated in electric evaporator 7, and by tungsten
10 capture of silk preenrichment device discharges again, and the aerosol containing atomic state zinc enters in carrier gas gas circuit 3 collaborates threeway 11, then with
The argon hydrogen gaseous mixture flowed out in auxiliary gas mass flowmenter 6 mixes in the threeway 11 of interflow, and mixed aerosol containing zinc passes through
Collaborate gas circuit 12 and enter torch pipe interface 13, enters back into inductive coupling plasma emission spectrograph 14.Solid sample feeding device most
Under the conditions of excellent, the range of linearity for surveying zinc is 0~2.5 μ g, and for the regression coefficient of standard curve 0.995 or more, the detection limit of zinc can
To reach 1pg, the relative standard deviation repeatedly measured is within 5%.
Embodiment two
By taking 5mg rice flour (national standard object GBW10045) as an example, use the argon hydrogen gaseous mixture containing 4% hydrogen as gas source, carrier gas
Mass flowmenter 4 is set as 700mL/min, with tungsten wire preenrichment device of the invention and electric evaporator and inductive coupling etc. from
The series connection of daughter emission spectrometer, other conditions are the same as example 1.The content of zinc is 14.9 ± 1.1 millis in 3 measurement samples
G kg, within 14.4 ± 0.8 mg/kg of standard value of the standard substance, the relative standard deviation of 7 measurements is
6.1%.
Embodiment three
By taking 2mg soil powder (national standard object GBW07401) as an example, use the argon hydrogen gaseous mixture containing 4% hydrogen as gas source,
Carrier gas mass flowmenter 4 is set as 700mL/min, with tungsten wire preenrichment device of the invention and electric evaporator and inductive coupling
Plasma emission spectrometer series connection, other conditions are the same as example 1.3 times measurement samples in zinc content be 694.5 ±
53.2 mg/kgs measure 7 relative standard deviations within 680 ± 25 mg/kg of standard value of the standard substance
It is 7.3%.
A kind of above-mentioned three explanations tungsten wire preenrichment device provided by the invention and electric evaporator and inductive coupling etc. from
Daughter emission spectrometer coupling arrangement, it is ensured that inductively coupled plasma emission spectrography surveys the stability of zinc, sensitivity
And accuracy.
Above embodiment be only preferred embodiments of the present invention will be described, not to the scope of the present invention into
Row limits, and without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to technical side of the invention
The various changes and improvements that case is made, should fall within the scope of protection determined by the claims of the present invention.
Claims (1)
1. a kind of measuring method for the tungsten wire preenrichment device for measuring zinc, characterized by the following steps:
A: 500 DEG C in air, by food samples to be measured dehydration, the ashing in navicular sample injector, remove most of organic substance；
B: carrier gas gas circuit is accurately mixed the argon hydrogen containing 2% -4% hydrogen of certain flow rate by carrier gas mass flowmenter
Gas is passed through electric evaporator, and ash residue is warming up to 1600 DEG C by electric evaporator, the aerosol containing zinc and tungsten wire evaporated
Tungsten wire contact in preenrichment device, wherein zinc is captured by tungsten wire；
C: under the argon hydrogen gaseous mixture atmosphere containing 2% -4% hydrogen, tungsten wire temperature is increased to 1800 DEG C by power socket, release
Zinc out enters interflow threeway with argon hydrogen gaseous mixture；
D: the argon hydrogen gaseous mixture containing 2% -4% hydrogen is passed through auxiliary gas mass flowmenter by auxiliary gas gas circuit, in interflow threeway
Collaborate with the zinc that tungsten wire preenrichment device comes out, enters torch pipe interface by collaborating gas circuit, enter back into inductively coupled plasma body
The content of emission spectrometer analysis zinc；The tungsten wire preenrichment device, by tungsten wire preenrichment device, electric heating evaporation device, torch
Interface tube, interflow threeway, carrier gas mass flowmenter, auxiliary gas mass flowmenter, diversion three-way, carrier gas gas circuit, auxiliary gas gas circuit
Composition, wherein the tungsten wire preenrichment device is made of tungsten wire, power socket and preenrichment device cavity；The carrier gas gas circuit and auxiliary
The right end gas access of gas gas circuit is helped to be connect by diversion three-way with argon hydrogen gaseous mixture gas source；The carrier gas gas circuit is sequentially connected shunting
Threeway, carrier gas mass flowmenter, electric heating evaporation device, tungsten wire preenrichment device, interflow threeway；The auxiliary gas gas circuit successively connects
Connect diversion three-way, auxiliary gas mass flowmenter, interflow threeway；The right end of the torch pipe interface passes through interflow gas circuit and interflow threeway
Connection, left end is connect with inductive coupling plasma emission spectrograph.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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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| US4833322A (en) * | 1986-05-02 | 1989-05-23 | Shell Oil Company | Method and apparatus for analysis of material |
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2015
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| US4833322A (en) * | 1986-05-02 | 1989-05-23 | Shell Oil Company | Method and apparatus for analysis of material |
| CN201732064U (en) * | 2010-07-15 | 2011-02-02 | 北京吉天仪器有限公司 | Electric heating evaporation atomic fluorescence spectrometer for measuring cadmium |
| CN102338745A (en) * | 2010-07-15 | 2012-02-01 | 北京吉天仪器有限公司 | Electro-thermal vaporization atomic fluorescence spectrometry method and spectrometer used for determining cadmium |
| CN102967590A (en) * | 2012-11-13 | 2013-03-13 | 北京吉天仪器有限公司 | Direct sample introduction type method and instrument for simultaneously measuring mercury and cadmium |
| CN204882366U (en) * | 2015-07-13 | 2015-12-16 | 中国农业科学院农业质量标准与检测技术研究所 | Emission spectrometry surveys pre -concentration tandem arrangement of zinc |
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