CN201522430U - Morphological analysis system of atomic fluorescence spectrometry gaseous arsenic compound - Google Patents
Morphological analysis system of atomic fluorescence spectrometry gaseous arsenic compound Download PDFInfo
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- CN201522430U CN201522430U CN2009201046399U CN200920104639U CN201522430U CN 201522430 U CN201522430 U CN 201522430U CN 2009201046399 U CN2009201046399 U CN 2009201046399U CN 200920104639 U CN200920104639 U CN 200920104639U CN 201522430 U CN201522430 U CN 201522430U
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Abstract
A morphological analysis system of an atomic fluorescence spectrometry gaseous arsenic compound is used to solve the problem of the analysis on morphology of gaseous arsenic compound. The technical plan of the utility model is that the morphological analysis system of the atomic fluorescence spectrometry gaseous arsenic compound comprises a standard generation or sample collection portion, a cryogenic trapping portion, a vacuum insulation separating pot, a hydrogen generation portion, an atomic fluorescence spectrometer and a signal recording portion, wherein an outlet of the sample collection portion is communicated with an inlet of the cryogenic trapping portion, the cryogenic trapping portion is provided with separation columns, outlets of the separation columns are communicated with an inlet of the atomic fluorescence spectrometer, an outlet of the hydrogen generation portion is communicated with the inlet of the atomic fluorescence spectrometer, the atomic fluorescence spectrometer signal is conveyed to the signal recording portion and then is output. The morphological analysis system has the advantages of ideal separation effect, good repeatability, high sensitivity, good linear correlation to the gaseous arsenic compound with different concentrations, wide linearity, good stability, low cost, simple operation and low analysis cost and the like.
Description
Technical field
The utility model relates to a kind of compound analysis device, especially for volatile gaseous arsenic compound AsH
3, CH
3AsH
2, (CH
3)
2AsH, (CH
3)
3The morphological analysis system of As belongs to the chemical detection analysis technical field.
Background technology
Arsenic is the environmental contaminants of severe toxicity, has a large amount of arsenic to discharge into environment, harm humans health in commercial production and geological movement.These inorganic arsenic or organoarsenium compounds that are released in the environment can be by the inorganic and organo-arsenic morphologization compound of series of physical chemistry and biological agent process generation different shape.What wherein, cause in the recent period that people pay attention to is can be converted into the bigger gaseous arsenic compound of toxicity in the biomass geochemistry cyclic process of arsenic.Compare with the arsenic compound of solubility, gaseous arsenic compound not only toxicity is stronger, and high volatility, is difficult to control, and health of human body is had bigger harm and disguise.So can be fast, sensitive, the accurate and cheap gaseous state arsenic analyzing and testing of carrying out is very necessary.The current method that is used for the arsenic compound analysis mainly comprises liquid chromatography-atomic fluorescence spectrophotometry coupling, liquid chromatography-atomic absorption spectrum coupling, liquid chromatography-inductivity coupled plasma mass spectrometry coupling etc.These pick-up units are effectively to the compartment analysis of solubility arsenic compound, analyzing and testing highly sensitive, technical method is ripe, stable.But the target compound of these above-mentioned technology must be a solution state, and can only carry out compartment analysis to solubility arsenic morphology compound.Though and only a few gaseous state arsenic analytical technology has report, analytical effect is unsatisfactory.Wherein the gas chromatography-mass spectrography report is used to the compartment analysis of gaseous arsenic compound, but because adopt the detecting device of non-exclusive, sensitivity is lower.Though the detection sensitivity of gas chromatography-inductivity coupled plasma mass spectrometry coupling and gas chromatography-mass spectrography specific sensitivity mutually are greatly improved, but instrument costs an arm and a leg, complicated operation, service condition requires high, is unfavorable for applying.
Summary of the invention
Technical problem to be solved in the utility model provides a kind of atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, to satisfy the requirement that fast, accurately reaches low-cost assay determination of gaseous arsenic compound form in the environmental sample.
The alleged problem of the utility model is solved by following technical scheme:
A kind of atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, its special feature is, it is generated or the sample collection part by standard, the cryogenic trapping part, the vacuum insulation separating tank, hydrogen generation part, atomic fluorescence spectrometer and signal record are partly formed, wherein, the sample collection section port partly enters the mouth with cryogenic trapping and is communicated with, cryogenic trapping partly is provided with separating column, this separating column outlet is communicated with the import of atomic fluorescence spectrometer, the import of the outlet connection atomic fluorescence spectrometer of part takes place in described hydrogen, and atomic fluorescence spectrometer signal conveys to signal record is partly exported.
Above-mentioned atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, described standard generation or sample collection device comprise the reaction vessel jar and the lid of PTFE material, lid is provided with solution of potassium borohydride pipeline, helium inlet and gas vent, the solution of potassium borohydride pipeline connects peristaltic pump, is provided with magnetic stir bar in the reaction vessel jar.
Above-mentioned atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, described cryogenic trapping device is made up of liquid nitrogen container and separating column, the separating column cylinder length 50-60cm of PTFE material, filling length in it is the absorbent cotton of 20-30cm, the absorbent cotton quality is 0.5-1.0g, cylinder external diameter 6.0mm, internal diameter 4.0mm, separating column is inserted in the liquid nitrogen container, makes to fill 3-5cm under the complete submergence liquid nitrogen liquid level of absorbent cotton part.
Above-mentioned atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, described hydrogen formation apparatus comprises Mixed liquid T-branch, is respectively equipped with aqueous slkali pipeline and acid solution pipeline, hydrogen pipeline, gas-carrier pipeline, auxiliary air pipe and the gas-liquid separator of peristaltic pump; Described Mixed liquid T-branch connects aqueous slkali pipeline, acid solution pipeline and one-level hydrogen pipeline respectively, described gas-carrier pipeline is communicated with the one-level hydrogen pipeline, the terminal one-level gas-liquid separator that is communicated with of one-level hydrogen pipeline, one-level gas-liquid separator gas vent pipeline is communicated with the secondary gas-liquid separator, auxiliary air pipe is communicated with one-level gas-liquid separator gas vent pipeline, and secondary gas-liquid separator gas vent pipeline is communicated with the atomizer inlet of separating column export pipeline, atomic fluorescence spectrometer.
The utility model to be sensitive at still lacking at present, gaseous arsenic compound analytical equipment problem fast and accurately, proposed a kind of simple to operate, with low cost, sensitive and accurate atomic fluorescence spectrophotometry morphological analysis system.This device utilizes the special efficacy detecting device of the cheap relatively atomic fluorescence spectrometer of cost as gaseous arsenic compound, and highly sensitive, selectivity is strong, technology maturation, stable performance; This device is simple, with low cost to process operations such as the capture of gaseous arsenic compound, separation, has avoided the use of large-scale chromatographic apparatus and chromatograph packing material; Utilize absorbent cotton and temperature control equipment to replace traditional chromatography packed column, greatly reduce the difficulty of analytical test; Because filling material adopts absorbent cotton, whole tripping device pipeline gaseous tension is very little, makes separating part be more prone to carry out on-line coupling with atomic fluorescence spectrophotometry, and the pipeline of having avoided the air pressure height to cause is simultaneously revealed.Experiment shows, adopt the utility model device, volatile gaseous arsenic compound for different shape can reach baseline separation in 3 minutes, separating effect ideal to gaseous arsenic compound, favorable reproducibility (n=7, relative standard deviation (RSD)≤8%), highly sensitive (detection limit DL is 0.005ng As), to variable concentrations gaseous arsenic compound linear dependence good (more than the r=0.99), the range of linearity wide (0.05ng-200ngAs), good stability, with low cost, simple to operate, analysis cost is low.
Description of drawings
Fig. 1 is the utility model structural representation.
Label is as follows in the accompanying drawing: 1. aqueous slkali pipeline, 2. acid solution pipeline, 3. Mixed liquid T-branch, 4. one-level hydrogen pipeline, 5. gas-carrier pipeline, 6. one-level gas-liquid separator, 7. one-level gas-liquid separator gas vent pipeline is 8. assisted air pipe, 9. secondary gas-liquid separator, 10. separating column export pipeline, 11. secondary gas-liquid separator gas vent pipelines, 12. atomic fluorescence spectrometer, 12-1. atomizer, 13. signal recording apparatus, 14. vacuum insulation separating tanks, 15. liquid nitrogen container, 16. separating column, 17. liquid nitrogen, 18. reaction vessel jars, 19. magnetic stir bar, 20. lid, 21. solution of potassium borohydride pipelines, 22. helium inlet, 23. gas vent, 24. peristaltic pumps.
Embodiment
Referring to Fig. 1, the utility model is generated by standard or sample collection part, cryogenic trapping part, vacuum insulation separating tank 14, hydrogen generation part, atomic fluorescence spectrometer 12 and signal record part 13 are formed, wherein standard generation sample collection section port partly enters the mouth with cryogenic trapping and is communicated with, cryogenic trapping partly is provided with separating column 16, this separating column outlet is communicated with the atomizer 12-1 inlet of atomic fluorescence spectrometer, the outlet that part takes place for described hydrogen is communicated with the import of atomic fluorescence spectrometer, the atomic fluorescence spectrometer signal conveys to and signal record partly export.
Still referring to Fig. 1, described standard generates or sample collection device can be that the sample culturing device also can be the gaseous arsenic compound gathering-device.It comprises the reaction vessel jar 18 and the lid 20 of PTFE material, lid is provided with solution of potassium borohydride pipeline 21, helium inlet 22 and gas vent 23, the solution of potassium borohydride pipeline connects peristaltic pump 24, be provided with magnetic stir bar 19 in the tank body, under the effect of magnetic stirring apparatus, hydride reacts stable more, rapid.
Still referring to Fig. 1, described cryogenic trapping device, form by liquid nitrogen container 15 and separating column 16, the separating column cylinder length 50-60cm of PTFE material, filling length in it is the absorbent cotton of 20-30cm, the absorbent cotton quality is 0.5-1.0g, cylinder external diameter 6.0mm, internal diameter 4.0mm, separating column insert in the liquid nitrogen container, make to fill 3-5cm under complete submergence liquid nitrogen 17 liquid levels of absorbent cotton part.Used separating column selects to have flexible PTFE material cylinder, and the filling material in the cylinder is an absorbent cotton.Described PTFE is a kind of (per) fluoropolymer that is made by tetrafluoroethene free radical polymerization, is a kind of crystalline polymer.PTFE has excellent chemical-resistant, and loss factor is low, stable performance, and good mechanical property, friction factor is low, and is nonflammable, has certain thermal adaptability scope, the material physicochemical property are stable.Another fundamental purpose of selecting this material for use be the PTFE tube Louis in bending, be convenient to be connected with the carrier gas gas circuit of atomic fluorescence spectrometer.The separating column inner stuffing is selected absorbent cotton for use, the agent structure of absorbent cotton is a cotton fiber, has strong polarity adsorptive power, has fluffy reticulate texture simultaneously, in the compound separation process, can play absorption simultaneously and resolve the effect of gaseous state arsenide and the intensification of stabilization column internal temperature, guarantee that gaseous arsenic compound reaches quick baseline separation.In addition, the selected atomic fluorescence spectrometer of the utility model needs the carrier gas of certain pressure, regime flow, if adopt the conventional chromatogram filler, line pressure is too high in cryogenic trapping and separating process, and the situation that carrier gas and separator leak takes place easily.Simultaneously, in the process that captures, air in the sample or other gas also have been trapped in the separation cylinder simultaneously, if captured gas on normal temperature or the higher temperature separating column, when gasifying, analyte is easy to generate big release air-flow of moment, water down the argon hydrogen stream, cause the argon hydrogen flame cancellation in the atomizer, greatly hinder the stability and the normal assay determination of system.Be seated in the vacuum insulation separating tank 14 after separating column captures and slowly heat up, gasification is slowly carried out to greatest extent, under the effect of carrier gas, steadily discharge and separate, both guaranteed separating effect and reappearance, kept the stability of atomizer argon-hydrogen flame again.
Still referring to Fig. 1, described hydrogen formation apparatus comprises Mixed liquid T-branch 3, be respectively equipped with the aqueous slkali pipeline 1 and the acid solution pipeline 2 that connect peristaltic pump, hydrogen pipeline 4, gas-carrier pipeline 5, auxiliary air pipe 8 and gas-liquid separator, described Mixed liquid T-branch connects the aqueous slkali pipeline respectively, the acid solution pipeline, with one-level hydrogen pipeline 4, described gas-carrier pipeline is communicated with the one-level hydrogen pipeline, the terminal one-level gas-liquid separator 6 that is communicated with of one-level hydrogen pipeline, one-level gas-liquid separator gas vent pipeline 7 is communicated with secondary gas-liquid separator 9, auxiliary air pipe is communicated with one-level gas-liquid separator gas vent pipeline, secondary gas-liquid separator gas vent pipeline 11 and separating column export pipeline 10, the atomizer 12-1 inlet of atomic fluorescence spectrometer 12 is communicated with.Atomic fluorescence spectrometer need be kept stable flame when measuring arsenic, Gaseous Hydrogen and the burning of carrier gas argon gas that described device utilizes hydrogenation to react and generates generate argon-hydrogen flame, to guarantee the required temperature and the energy of atomization of arsenic.In hydrogenation reacts, feed the reductive agent solution of potassium borohydride in the aqueous slkali pipeline 1, feed dilute hydrochloric acid solution in the acid solution pipeline 2, both react and generate a large amount of Gaseous Hydrogens, hydrogen mixes the back and generates argon-hydrogen flame in atomizer 12-1 burning with argon gas, for the atomization of arsenic compound provides condition.The atomizer that gaseous arsenic compound after the separation is brought atomic fluorescence spectrometer into carrier gas carries out atomization, under the exciting of hollow cathode lamp, sends fluorescence, through the signal Processing and the amplification of photomultiplier, at last by 13 outputs of signal record part.
Still, utilize the utility model above-mentioned as follows: with 4%KBH to volatile gaseous arsenic compound assay determination process referring to Fig. 1
4(0.3%KOH) and 10%HCl (v/v) feeds aqueous slkali pipeline 1 respectively, 2, two kinds of solution of acid solution pipeline are written into Mixed liquid T-branch 3 by pipeline, at this, acid-base solution mixes and hydrogenation takes place reacts, and produces a large amount of Gaseous Hydrogens and waste liquid.The hydrogen that generates is brought into one-level gas-liquid separator 6 with carrier gas in the gas-carrier pipeline 5, and gas-liquid reaches to greatest extent separates.Gaseous Hydrogen is brought into secondary gas-liquid separator 9 again with carrier gas, enters the gas of secondary gas-liquid separator, under auxiliary air pipe 8 auxiliary gas effects, steadily enters atomizer 12-1 burning.Simultaneously, add a certain amount of different shape arsenic compound in reaction vessel jar 18, the oxalic acid that adds 5mL5% subsequently is as reaction medium and reaction reagent, 5%KBH
4Solution is pumped in the reaction vessel jar by the solution of potassium borohydride pipeline, and through the reaction of 5-6min, the gaseous arsenic compound standard of generation all is captured, is condensate on the separating column 16 under the stirring of magnetic stir bar 19.After capturing fully, separating column is transferred to vacuum insulation separating tank 14 and slowly heats up, the separating column carrier gas inlet connects standard and generates or the sample collection part, the separating column gas vent is communicated with the atomizer of atomic fluorescence spectrometer through threeway, gaseous arsenic compound successively enters atomic fluorescence spectrometer in separated back and detects, and testing result is by the signal recording apparatus record.Gaseous arsenic compound AsH
3, CH
3AsH
2, (CH
3)
2AsH, (CH
3)
3A can reach baseline separation in 3min.
Claims (4)
1. atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis system, it is characterized in that, it is generated or the sample collection part by standard, the cryogenic trapping part, vacuum insulation separating tank (14), hydrogen generation part, atomic fluorescence spectrometer (12) and signal record part (13) are formed, wherein the sample collection section port partly enters the mouth with cryogenic trapping and is communicated with, cryogenic trapping partly is provided with separating column (16), this separating column outlet is communicated with the import of atomic fluorescence spectrometer, the import of the outlet connection atomic fluorescence spectrometer of part takes place in described hydrogen, and the atomic fluorescence spectrometer signal output part is connected to the signal input part of signal record part.
2. atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis according to claim 1 system, it is characterized in that, described standard generation or sample collection portion branch comprise the reaction vessel jar (18) and the lid (20) of PTFE material, described lid is provided with solution of potassium borohydride pipeline (21), helium inlet (22) and gas vent (23), the solution of potassium borohydride pipeline connects peristaltic pump (24), is provided with magnetic stir bar (19) in the reaction vessel jar.
3. atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis according to claim 2 system, it is characterized in that, described cryogenic trapping part is made up of liquid nitrogen container (15) and separating column (16), described separating column cylinder length 50-60cm, filling length in it is the absorbent cotton of 20-30cm, the absorbent cotton quality is 0.5-1.0g, cylinder external diameter 6.0mm, internal diameter 4.0mm, separating column insert in the liquid nitrogen container, fill absorbent cotton and are immersed in 3-5cm under liquid nitrogen (17) liquid level fully.
4. according to claim 1 or 2 or 3 described atomic fluorescence spectrophotometry gaseous arsenic compound morphological analysis systems, it is characterized in that, described hydrogen generating unit branch comprises Mixed liquid T-branch (3), be respectively equipped with the aqueous slkali pipeline (1) and the acid solution pipeline (2) of peristaltic pump, hydrogen pipeline, gas-carrier pipeline (5), auxiliary air pipe (8) and gas-liquid separator, described Mixed liquid T-branch connects the aqueous slkali pipeline respectively, acid solution pipeline and one-level hydrogen pipeline (4), described gas-carrier pipeline is communicated with the one-level hydrogen pipeline, the terminal one-level gas-liquid separator (6) that is communicated with of one-level hydrogen pipeline, one-level gas-liquid separator gas vent pipeline (7) is communicated with secondary gas-liquid separator (9), auxiliary air pipe is communicated with one-level gas-liquid separator gas vent pipeline, secondary gas-liquid separator gas vent pipeline (11) and separating column export pipeline (10), atomizer (12-1) inlet of atomic fluorescence spectrometer (12) is communicated with.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009201046399U CN201522430U (en) | 2009-09-14 | 2009-09-14 | Morphological analysis system of atomic fluorescence spectrometry gaseous arsenic compound |
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|---|---|---|---|
| CN2009201046399U CN201522430U (en) | 2009-09-14 | 2009-09-14 | Morphological analysis system of atomic fluorescence spectrometry gaseous arsenic compound |
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| CN201522430U true CN201522430U (en) | 2010-07-07 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104280381A (en) * | 2013-07-01 | 2015-01-14 | 北京瑞利分析仪器有限公司 | Device saving potassium borohydride using amount of atomic fluorescence spectrometer |
| CN109001171A (en) * | 2018-08-15 | 2018-12-14 | 东北大学 | A kind of atomic fluorescence method monitors the device and method of nitrogen nutrition salt in ambient water |
-
2009
- 2009-09-14 CN CN2009201046399U patent/CN201522430U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104280381A (en) * | 2013-07-01 | 2015-01-14 | 北京瑞利分析仪器有限公司 | Device saving potassium borohydride using amount of atomic fluorescence spectrometer |
| CN109001171A (en) * | 2018-08-15 | 2018-12-14 | 东北大学 | A kind of atomic fluorescence method monitors the device and method of nitrogen nutrition salt in ambient water |
| CN109001171B (en) * | 2018-08-15 | 2020-10-09 | 东北大学 | Device and method for monitoring nitrogen nutritive salt in environmental water by atomic fluorescence method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100707 Termination date: 20120914 |