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
- Publication number
- CN104990910A CN104990910A CN201510409052.9A CN201510409052A CN104990910A CN 104990910 A CN104990910 A CN 104990910A CN 201510409052 A CN201510409052 A CN 201510409052A CN 104990910 A CN104990910 A CN 104990910A
- Authority
- CN
- China
- Prior art keywords
- gas
- zinc
- tungsten filament
- preenrichment
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000011701 zinc Substances 0.000 title claims abstract description 49
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 49
- 238000004993 emission spectroscopy Methods 0.000 title claims abstract description 6
- 238000004458 analytical method Methods 0.000 title abstract description 9
- 238000004094 preconcentration Methods 0.000 title abstract 8
- 239000007789 gas Substances 0.000 claims abstract description 85
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 46
- 239000010937 tungsten Substances 0.000 claims abstract description 46
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012159 carrier gas Substances 0.000 claims abstract description 25
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 230000008878 coupling Effects 0.000 claims abstract description 19
- 238000010168 coupling process Methods 0.000 claims abstract description 19
- 238000005859 coupling reaction Methods 0.000 claims abstract description 19
- 230000001939 inductive effect Effects 0.000 claims abstract description 13
- 238000004380 ashing Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 238000005485 electric heating Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 235000013305 food Nutrition 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 1
- 239000007787 solid Substances 0.000 abstract description 17
- 238000005070 sampling Methods 0.000 abstract description 13
- 238000009616 inductively coupled plasma Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000008016 vaporization Effects 0.000 abstract 2
- 238000009834 vaporization Methods 0.000 abstract 2
- 239000000443 aerosol Substances 0.000 abstract 1
- 230000029087 digestion Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 229910052793 cadmium Inorganic materials 0.000 description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 229910052753 mercury Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 2
- 238000003705 background correction Methods 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000000608 laser ablation Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000010584 magnetic trap Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000286209 Phasianidae Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 238000001675 atomic spectrum Methods 0.000 description 1
- 235000008452 baby food Nutrition 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000246 remedial effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510409052.9A CN104990910B (en) | 2015-07-13 | 2015-07-13 | A kind of emission spectrometry surveys the preenrichment tandem arrangement and analysis method of zinc |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510409052.9A CN104990910B (en) | 2015-07-13 | 2015-07-13 | A kind of emission spectrometry surveys the preenrichment tandem arrangement and analysis method of zinc |
Publications (2)
Publication Number | Publication Date |
---|---|
CN104990910A true CN104990910A (en) | 2015-10-21 |
CN104990910B CN104990910B (en) | 2018-12-21 |
Family
ID=54302749
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510409052.9A Expired - Fee Related CN104990910B (en) | 2015-07-13 | 2015-07-13 | A kind of emission spectrometry surveys the preenrichment tandem arrangement and analysis method of zinc |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104990910B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
-
2015
- 2015-07-13 CN CN201510409052.9A patent/CN104990910B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Non-Patent Citations (2)
Title |
---|
HIDEO HAYASHI等: "Electrothermal Vaporization on a Tungsten Filament for the Determination of Arsenic in Chloride Solutions by Low-Pressure Helium ICP-MS", 《ANALYTICAL SCIENCES》 * |
张晓红等: "固体进样原子荧光测量农产品中的镉", 《现代科学仪器》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
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 |
Also Published As
Publication number | Publication date |
---|---|
CN104990910B (en) | 2018-12-21 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Machado et al. | Solid sampling: advantages and challenges for chemical element determination—a critical review | |
CN104849118B (en) | A kind of inductively coupled plasma mass spectrometer coupling interface device and analysis method | |
Beauchemin | Environmental analysis by inductively coupled plasma mass spectrometry | |
Oviedo et al. | Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry | |
Feist et al. | Preconcentration of some metal ions with lanthanum-8-hydroxyquinoline co-precipitation system | |
Paul et al. | Mineral assay in atomic absorption spectroscopy | |
Bakirdere et al. | From mg/kg to pg/kg levels: a story of trace element determination: a review | |
Virgilio et al. | Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants | |
Wen et al. | A new coupling of ionic liquid based-single drop microextraction with tungsten coil electrothermal atomic absorption spectrometry | |
Dantas et al. | The combination of infrared and microwave radiation to quantify trace elements in organic samples by ICP OES | |
Frentiu et al. | New method for mercury determination in microwave digested soil samples based on cold vapor capacitively coupled plasma microtorch optical emission spectrometry: comparison with atomic fluorescence spectrometry | |
Picoloto et al. | Determination of inorganic pollutants in soil after volatilization using microwave-induced combustion | |
Oliveira et al. | Development of methods for the determination of cadmium and thallium in oil shale by-products with graphite furnace atomic absorption spectrometry using direct analysis | |
Sadiq et al. | Solid sampling ETV-ICPOES coupled to a nebulization/pre-evaporation system for direct elemental analysis of glutinous rice by external calibration with standard solutions | |
Zaksas et al. | Solid sampling in analysis of animal organs by two-jet plasma atomic emission spectrometry | |
CN204882366U (en) | Emission spectrometry surveys pre -concentration tandem arrangement of zinc | |
Mao et al. | Simultaneous trapping of Zn and Cd by a tungsten coil and its application to grain analysis using electrothermal inductively coupled plasma mass spectrometry | |
Duan et al. | Direct determination of arsenic in soil samples by fast pyrolysis–chemical vapor generation using sodium formate as a reductant followed by nondispersive atomic fluorescence spectrometry | |
CN104990910A (en) | Pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and analysis method | |
Lan et al. | Rapid and sensitive determination of Se and heavy metals in foods using electrothermal vaporization inductively coupled plasma mass spectrometry with a novel transportation system | |
Lv et al. | Portable and miniature mercury analyzer using direct sampling inbuilt-metal ceramic electrothermal vaporization | |
Welna et al. | Ultrasound-and microwave-assisted extractions followed by hydride generation inductively coupled plasma optical emission spectrometry for lead determination in geological samples | |
Frentiu et al. | Application of low-cost electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry for simultaneous determination of Cd and Pb in environmental samples | |
CN104977193B (en) | In a kind of infant food and dairy products the sample-pretreating method of detection of content of element and use its detection method | |
Yin et al. | Determination of trace rare earth elements in environmental samples by low temperature electrothermal vaporization inductively coupled plasma mass spectrometry after synergistic extraction with dimethylheptyl methyl phosphate and 1-phenyl-3-methyl-4-benzoyl-pyrazalone-5 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181221 |