CN204679320U - A kind of inductively coupled plasma mass spectrometer coupling interface device - Google Patents
A kind of inductively coupled plasma mass spectrometer coupling interface device Download PDFInfo
- Publication number
- CN204679320U CN204679320U CN201520348710.3U CN201520348710U CN204679320U CN 204679320 U CN204679320 U CN 204679320U CN 201520348710 U CN201520348710 U CN 201520348710U CN 204679320 U CN204679320 U CN 204679320U
- Authority
- CN
- China
- Prior art keywords
- inductively coupled
- coupled plasma
- mass spectrometer
- gas
- interface device
- 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.)
- Expired - Fee Related
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The utility model provides a kind of inductively coupled plasma mass spectrometer coupling interface device measuring cadmium in foods, and described inductively coupled plasma mass spectrometer coupling interface device comprises: torch interface tube, carrier gas mass flowmeter, assisted gas mass flowmeter, diversion three-way, interflow threeway, carrier gas channel, assisted gas pipeline etc.This apparatus structure is simple, solves tungsten filament and catches electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling used time plasma puts out the low difficult problem of torch, jitter and sensitivity.The utility model has the advantage of without the need to clearing up process to food samples, the detection to wherein Determination of Trace Amount Cadmium can be realized that there is the features such as direct, quick, highly sensitive, good stability.
Description
Technical field
The utility model belongs to field of detection of food safety, relates to a kind of inductively coupled plasma mass spectrometer coupling interface device measuring cadmium in foods.
Technical background
Current, China's some areas agricultural environment and agricultural product heavy metal cadmium problem comparatively outstanding.In April, 2014, cadmium is classified as the primary pollutant of soil environment by Environmental Protection Department combines issue " national Soil Pollution Investigation publication " with Ministry of Land and Resources.Cadmium in agricultural environment can be accumulated in edible portion by Crop, and is enriched in livestock and poultry and aquatic products by food chain, thus finally enters into generation harm in consumer's body.After Hunan " cadmium rice " event in 2013, in agricultural product, the pollution problem of cadmium is consumer and media spotlight always, and at present the cadmium pollution situation of agricultural product allows of no optimist really, wherein the pollution condition such as grain, vegetables, tealeaves, pluck, aquatic products is comparatively outstanding.
At present, measure the instrument of cadmium 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 5009.15-2003 " mensuration of cadmium in foods ", SN/T 2056-2008 " imports and exports in tealeaves plumbous, arsenic, cadmium, copper, the mensuration ICP-AES of iron content ", SB/T 10922-2012 " chromium in meat quail, copper, total arsenic, cadmium, total mercury, plumbous mensuration inductively coupled plasma mass spectrometry " 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-MS is because its antijamming capability is comparatively strong, linear dynamic range is wide and the ability of Simultaneous multi element analysis, and in solid sampling spectral technique, extremely researcher pays close attention to.
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.Wherein, the novel solid sampling technique that cadmium solid sample feeding device is China scientific research personnel exploitation in recent years caught by the tungsten filament published, tungsten filament can catch atomic state cadmium at normal temperatures, and at high temperature effectively can discharge cadmium, then can realize preenrichment and Matrix separation two targets by catching of cadmium with Matrix separation, thus effectively alleviate Matrix effects.Simultaneously, this solid sample feeding device utilizes porous carbon as electric heating evaporation material, stability and the graphite-pipe of porous carbon materials are close, but evaporation power consumption is far below the latter, add that porous carbon materials self space is comparatively large, rapid heat dissipation, therefore can realize simple air-cooled fast but not water-cooled, be easy to miniaturization.At present, the survey cadmium solid sample feeding device of above-mentioned technology is utilized to achieve and the connecting of AFS.Solid sample feeding device in prior art, main function components comprises online cineration device, electric heating evaporation parts and tungsten filament capturing means, and when sample is in ashing state, the gas circuit of electric heating evaporation parts is open; When sample complete ashing enter electric heating evaporation parts time, the gas circuit of electric heating evaporation parts is closed.Because the gas circuit folding of electric heating evaporation parts and switching can cause the cataclysm of whole gas circuit air-flow and air pressure, the impact of this signals collecting for AFS is little, but for comparatively responsive plasma torch flame, swinging of signal can be caused even to put out torch; Meanwhile, in original argon hydrogen combination gas, hydrogen volume is not suitable for ICP-MS than the carrier gas atmosphere more than 10%, and the too high meeting of density of hydrogen causes putting out torch due to a large amount of ionization energy of hydrogen consumption.Therefore, original tungsten filament for AFS is caught its connecting interface of solid sample feeding device, gas circuit and atmosphere thereof and is formed and be not suitable for ICP-MS, if be directly connected with ICP-MS, ICP-MS can be caused normally to work, thus stable, the Accurate Determining of cadmium in foods cannot be realized.
Summary of the invention
The purpose of this utility model is for the problems referred to above, a kind of tungsten filament is provided to catch electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling connection device, this apparatus structure is simple, solve tungsten filament and catch electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling used time plasma puts out the low difficult problem of torch, jitter and sensitivity, without the need to clearing up process to food samples, the detection to wherein Determination of Trace Amount Cadmium can be realized, there is the features such as direct, quick, highly sensitive, good stability.
A kind of inductively coupled plasma mass spectrometer coupling interface device measuring cadmium in foods, described inductively coupled plasma mass spectrometer coupling interface device is made up of torch interface tube (13), carrier gas mass flowmeter (5), assisted gas mass flowmeter (6), diversion three-way (2), interflow threeway (11), carrier gas channel (3), assisted gas pipeline (4), it is characterized in that: described carrier gas channel (3) is connected with argon hydrogen combination gas source of the gas (1) by diversion three-way (2) with the bottom righthand side gas access of assisted gas pipeline (4).
Described carrier gas channel (3) connects diversion three-way (2), carrier gas mass flowmeter (5), solid sample feeding device (7), interflow threeway (11) successively.
Described assisted gas pipeline (4) connects diversion three-way (2), assisted gas mass flowmeter (6), interflow threeway (11) successively.
Described carrier gas mass flowmeter (5) right-hand member connects diversion three-way (2) outlet, and left end connects solid sample feeding device (7).
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 icp ms (14).
Described carrier gas channel (3), assisted gas pipeline (4), interflow gas circuit (12) pipeline, torch interface tube (13) are teflon material.
The analytical approach of described inductively coupled plasma mass spectrometer coupling interface device, comprises the steps:
About a, in atmosphere 500 DEG C, food samples to be measured dewaters by online ashing parts (8), ashing, removes most of organic substance;
B, described carrier gas channel (3) are by carrier gas mass flowmeter (5), is that the argon hydrogen combination gas of 2%-4% hydrogen passes into solid sample feeding device (7) accurately by certain flow rate containing volume ratio, ash residue is warming up to about 1600 DEG C by electric heating evaporation parts (9), the tungsten wire contact containing cadmium gasoloid and tungsten filament capturing means (10) obtained, wherein cadmium is caught by tungsten filament;
C, under the argon hydrogen combination gas atmosphere containing volume ratio being 2%-4% hydrogen, tungsten filament temperature is elevated to 1600-2000 DEG C by tungsten filament capturing means (10), and the cadmium discharged enters interflow threeway (11) with argon hydrogen combination gas;
The argon hydrogen combination gas containing volume ratio being 2%-4% hydrogen is passed into assisted gas mass flowmeter (6) by d, assisted gas pipeline (4), collaborate with tungsten filament capturing means (10) cadmium out at interflow threeway (11), enter torch interface tube (13) by interflow gas circuit (12), then enter the content that icp ms (14) analyzes cadmium.
The beneficial effect of the invention:
1, the bottleneck difficult problem that tungsten filament catches electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling is solved---stable plasma torch flame, overcomes because tungsten filament catches that electric heating evaporation solid sample feeding device connects and the airflow fluctuation that causes makes the plasma torch flame of icp ms to stop working problem and signal sensitivity step-down 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; Secondary air, while stable plasma torch flame, fully can carry the cadmium in gas circuit dead volume, add transfer efficiency, improve sensitivity for analysis.
Accompanying drawing illustrates:
Below with reference to accompanying drawing and instantiation, the present invention will be further elaborated.
Fig. 1-catch electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling connection device for tungsten filament;
1--argon hydrogen combination gas source of the gas, 2--diversion three-way, 3--carrier gas channel, 4--assisted gas pipeline, 5--carrier gas mass flowmeter, 6--assisted gas mass flowmeter, 7--solid sample feeding device, the online ashing parts of 8--, 9--electric heating evaporation parts, 10--tungsten filament capturing means, 11--collaborates threeway, 12--collaborates gas circuit, and 13--torch interface tube, 14--is connected into icp ms.
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 1
The utility model provides a kind of tungsten filament to catch electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling connection device, embodiment comprises torch interface tube (13), carrier gas mass flowmeter (5), assisted gas mass flowmeter (6), diversion three-way (2), interflow threeway (11), carrier gas channel (3), assisted gas pipeline (4) forms, wherein: described carrier gas channel (3) is connected with argon hydrogen combination gas source of the gas (1) by diversion three-way (2) with the bottom righthand side gas access of assisted gas pipeline (4), described carrier gas channel (3) connects diversion three-way (2) successively, carrier gas mass flowmeter (5), solid sample feeding device (7), interflow threeway (11), described assisted gas pipeline (4) connects diversion three-way (2) successively, assisted gas mass flowmeter (6), interflow threeway (11), described carrier gas mass flowmeter (5) right-hand member connects diversion three-way (2) outlet, and left end connects solid sample feeding device (7).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 icp ms (14).
When the standard solution containing cadmium is before electric heating evaporation solid sample feeding device sample introduction caught by tungsten filament, the dividing potential drop of argon hydrogen combination gas source of the gas (1) containing 2% hydrogen is set in about 0.5Mpa, carrier gas mass flowmeter (5) is set as 800mL/min, assisted gas mass flowmeter (6) is set as 300mL/min, cadmium is evaporated by electric heating evaporation parts (9) in solid sample feeding device (7), and caught by tungsten filament capturing means (10) and discharge again, gasoloid containing atomic state cadmium enters interflow threeway (11) in carrier gas channel (3), collaborating to mix in threeway (11) with the argon hydrogen combination gas flowed out in assisted gas mass flowmeter (6) again, the mixed cadmium gasoloid that contains enters torch interface tube (13) by interflow gas circuit (12), enter icp ms (14) again.Under electric heating evaporation solid sample feeding device optimal conditions caught by tungsten filament, the range of linearity surveying cadmium is 0.1 pik ~ 800 nanogram, the regression coefficient of typical curve is more than 0.996, and the detection limit of cadmium can reach 0.1 pik, and the relative standard deviation repeatedly measured is within 4%.
Embodiment 2
For 5 milligrams of ground rice (GB thing GBW10043), use the argon hydrogen combination gas containing 4% hydrogen as source of the gas, carrier gas mass flowmeter (5) is set as 700mL/min, assisted gas mass flowmeter (6) is set as 300mL/min, catch electric heating evaporation solid sample feeding device and icp ms with coupling arrangement series connection tungsten filament of the present invention, other conditions are identical with embodiment one.In working sample cadmium be 9.8 ± 0.6 micrograms/kilogram, this standard substance standard value 12 ± 3 microgram/kilogram within, the relative standard deviation repeatedly measured is within 10%, and the recovery of standard addition of high, medium and low (0.1,0.8,2.0 nanogram) level is all 85% ~ 110%.
Embodiment 3
For 5 milligrams of scallop powder (GB thing GBW10024), use the argon hydrogen combination gas containing 3% hydrogen as source of the gas, carrier gas mass flowmeter (5) is set as 700mL/min, assisted gas mass flowmeter (6) is set as 300mL/min, catch electric heating evaporation solid sample feeding device and icp ms with coupling arrangement series connection tungsten filament of the present invention, other conditions are identical with embodiment one.In working sample cadmium be 971.6 ± 33.7 micrograms/kilogram, this standard substance standard value 1060 ± 100 microgram/kilogram within, the relative standard deviation repeatedly measured is within 10%, the recovery of standard addition of high, medium and low (0.1,0.8,2.0 nanogram) level all 83% be 9.8 ± 0.6 micrograms/kilogram, this standard substance standard value 12 ± 3 microgram/kilogram within, the relative standard deviation repeatedly measured is within 10%, and the recovery of standard addition of high, medium and low (0.1,0.8,2.0 nanogram) level is all 85% ~ 110%.
Above-mentioned three examples illustrate that a kind of tungsten filament that the utility model provides catches electric heating evaporation solid sample feeding device and inductively coupled plasma mass spectrometer coupling connection device, can ensure the stability of inductivity coupled plasma mass spectrometry survey cadmium, sensitivity and accuracy.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (6)
1. an inductively coupled plasma mass spectrometer coupling interface device, described inductively coupled plasma mass spectrometer coupling interface device is made up of torch interface tube (13), carrier gas mass flowmeter (5), assisted gas mass flowmeter (6), diversion three-way (2), interflow threeway (11), carrier gas channel (3), assisted gas pipeline (4), it is characterized in that: described carrier gas channel (3) is connected with argon hydrogen combination gas source of the gas (1) by diversion three-way (2) with the bottom righthand side gas access of assisted gas pipeline (4).
2. inductively coupled plasma mass spectrometer coupling interface device as claimed in claim 1, is characterized in that: described carrier gas channel (3) connects diversion three-way (2), carrier gas mass flowmeter (5), solid sample feeding device (7), interflow threeway (11) successively.
3. inductively coupled plasma mass spectrometer coupling interface device as claimed in claim 1 or 2, is characterized in that: described assisted gas pipeline (4) connects diversion three-way (2), assisted gas mass flowmeter (6), interflow threeway (11) successively.
4. inductively coupled plasma mass spectrometer coupling interface device as claimed in claim 1 or 2, it is characterized in that: described carrier gas mass flowmeter (5) right-hand member connects diversion three-way (2) outlet, and left end connects solid sample feeding device (7).
5. inductively coupled plasma mass spectrometer coupling interface device as claimed in claim 1 or 2, it is characterized in that: 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 icp ms (14).
6. inductively coupled plasma mass spectrometer coupling interface device as claimed in claim 1 or 2, is characterized in that: described carrier gas channel (3), assisted gas pipeline (4), interflow gas circuit (12) pipeline, torch interface tube (13) are teflon material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520348710.3U CN204679320U (en) | 2015-05-26 | 2015-05-26 | A kind of inductively coupled plasma mass spectrometer coupling interface device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520348710.3U CN204679320U (en) | 2015-05-26 | 2015-05-26 | A kind of inductively coupled plasma mass spectrometer coupling interface device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204679320U true CN204679320U (en) | 2015-09-30 |
Family
ID=54179003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520348710.3U Expired - Fee Related CN204679320U (en) | 2015-05-26 | 2015-05-26 | A kind of inductively coupled plasma mass spectrometer coupling interface device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204679320U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849118A (en) * | 2015-05-26 | 2015-08-19 | 中国农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometer coupling interface device and analysis method |
-
2015
- 2015-05-26 CN CN201520348710.3U patent/CN204679320U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849118A (en) * | 2015-05-26 | 2015-08-19 | 中国农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometer coupling interface device and analysis method |
| CN104849118B (en) * | 2015-05-26 | 2018-05-01 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of inductively coupled plasma mass spectrometer coupling interface device and analysis method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104849118A (en) | Inductively coupled plasma mass spectrometer coupling interface device and analysis method | |
| Davidson | Methods for the determination of heavy metals and metalloids in soils | |
| Li et al. | Determination of As and Se in coal and coal combustion products using closed vessel microwave digestion and collision/reaction cell technology (CCT) of inductively coupled plasma mass spectrometry (ICP-MS) | |
| Fan et al. | Dithizone–chloroform single drop microextraction system combined with electrothermal atomic absorption spectrometry using Ir as permanent modifier for the determination of Cd in water and biological samples | |
| Pohl et al. | Chemical-vapor generation of transition metals through the reaction with tetrahydroborate in recent achievements in analytical atomic spectrometry | |
| Jankowski et al. | Multielement determination of heavy metals in water samples by continuous powder introduction microwave-induced plasma atomic emission spectrometry after preconcentration on activated carbon | |
| CN103604686B (en) | The pre-treatment of rapid determination of content of cadmium element and quantitative analysis method in a kind of Fast Measurement rice | |
| Fırat et al. | Vortex-assisted switchable liquid-liquid microextraction for the preconcentration of cadmium in environmental samples prior to its determination with flame atomic absorption spectrometry | |
| CN103698316B (en) | A kind of iron ore multielement synchronization detecting method of sensitive reliable, fast and stable | |
| Boschetti et al. | Sequential and simultaneous determination of four elements in soil samples using high-resolution continuum source graphite furnace atomic and molecular absorption spectrometry | |
| Rezende et al. | Quantification and speciation of mercury in streams and rivers sediment samples from Paracatu, MG, Brazil, using a direct mercury analyzer® | |
| Butler et al. | Atomic spectrometry update–a review of advances in environmental analysis | |
| Lv et al. | Portable and miniature mercury analyzer using direct sampling inbuilt-metal ceramic electrothermal vaporization | |
| Angyus et al. | Interference-free, green microanalytical method for total mercury and methylmercury determination in biological and environmental samples using small-sized electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry | |
| Belarra et al. | Direct determination of cobalt and zinc in samples of different volatility by means of solid sampling–graphite furnace atomic absorption spectrometry | |
| CN204679320U (en) | A kind of inductively coupled plasma mass spectrometer coupling interface device | |
| Frentiu et al. | Determination of total mercury in fish tissue using a low-cost cold vapor capacitively coupled plasma microtorch optical emission microspectrometer: comparison with direct mercury determination by thermal decomposition atomic absorption spectrometry | |
| Anderson et al. | Sequential hydride generation/pneumatic nebulisation inductively coupled plasma mass spectrometry for the fractionation of arsenic and selenium species | |
| Pancras et al. | Multi-element electrothermal AAS determination of 11 marker elements in fine ambient aerosol slurry samples collected with SEAS-II | |
| Xue et al. | Determination of Hg, As, Pb, and Cd in orchard soils by sequential injection vapor generation atomic fluorescence spectrometry | |
| Kheamphet et al. | A simple and cost-effective smartphone-based digital imaging device for the quantification of selected heavy metals in Thai rice | |
| Frank et al. | Direct determination of arsenic in acid digests of plant and peat samples using HG-AAS and ICP-SF-MS | |
| 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 | |
| Aydin et al. | Chemical speciation of vanadium in coal bottom ash | |
| Luo | Determination of total arsenic in wastewater and sewage sludge samples by using hydride-generation atomic fluorescence spectrometry under the optimized analytical conditions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150930 Termination date: 20160526 |