CN201701756U - Device for separating valence chromium by temperature rise - Google Patents
Device for separating valence chromium by temperature rise Download PDFInfo
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- CN201701756U CN201701756U CN2010202191797U CN201020219179U CN201701756U CN 201701756 U CN201701756 U CN 201701756U CN 2010202191797 U CN2010202191797 U CN 2010202191797U CN 201020219179 U CN201020219179 U CN 201020219179U CN 201701756 U CN201701756 U CN 201701756U
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Abstract
The utility model relates to a device for separating valence chromium by temperature rise, which belongs to the technical field of separation detection and is characterized by comprising a sample bearing mechanism, a heating mechanism and an inert gas protection mechanism, wherein the heating device is arranged opposite to the sample bearing mechanism and is used for directly or indirectly heating the sample bearing mechanism; the inert gas protection mechanism is arranged outside the sample bearing mechanism; and the inert gas protection mechanism is provided with an inert gas vent. The utility model has the advantages of simple structure, compact assembly, convenient operation, economy and practicability, good generality, wide application range, good selection effect, high separation efficiency, accurate measurement and the like and can be widely applied to carrying out separation detection on trivalent chromium and hexavalent chromium.
Description
Technical field
The utility model belongs to and separates the detection technique field, particularly relates to a kind of the intensification and separates the device of valence state chromium.
Background technology
Chromium Cr is the metallic element that often touches in the daily life, there are two kinds of valence states of sexavalence and trivalent, be expressed as Cr VI (Cr (VI)) and trivalent chromium (Cr (III)) respectively, wherein Cr (VI) is strong carcinogenic substance, Cr (III) is then to the human body beneficial, so be necessary very much Cr (III) and Cr (VI) in the specimen.But effectively separation of C r (III) and Cr (VI) are the technical barrier problems of fine solution of failing at present.
At present, Cr (III) commonly used and the separation method of Cr (VI) have two kinds of colorimetric method and ion-exchanges, and the colorimetric method cross reaction is many, and selectivity is bad; Ion-exchange is complex operation comparatively, and is vulnerable to the interference of other ion and organic complexing agent, and separating effect is not good.There is the equipment complexity in prior art, complex operation, and the cost height, poor selectivity, separative efficiency is low, measures technical problems such as inaccurate.
Summary of the invention
The utility model provides a kind of the intensification to separate the device of valence state chromium for solving the technical problem that exists in the known technology.
The purpose of this utility model provides a kind of simple in structure, and assembling is compact, and easy to operate, economical and practical, versatility is good, and applied range is selected effectively, and the separative efficiency height is measured the device of the intensification separation valence state chromium of characteristics such as accurate.
The utility model adopts programmed temperature method separation of C r (III) and Cr (VI), be to utilize Cr (III) to form the stronger complex compound of volatilization with plug fen formyl trifluoroacetone (TTA), can carry out the new method that Cr (III) separates with Cr (VI) at a lower temperature by the principle that steams and separate with Cr (VI).The instrument that Cr (III) separates with Cr (VI) is made up of automatic pre-treatment, sampling device and temperature programming separator, wherein automatically pre-treatment, sampling device be one can realize heating and the automatic sampler of jolting (wherein heating can be by the solid heat block realization of water-bath or graphite or aluminium; Finish the generation of Cr (III) complex compound therein and it is carried in the temperature programming separator automatically, load mode can adopt syringe pump to finish.The temperature programming separator comprise a heating element heater and sample bogey (the sample bogey can be can spontaneous heating tungsten boat or carbon boat, unite two into one with heater this moment; Also can be quartz boat or the ceramic boat that self can not generate heat, this moment, heater can be a tube furnace, by temperature programming at a lower temperature (500 ℃-800 ℃, keep 50-100 second) complex compound of Cr (III) is steamed and separates with Cr (VI).
The technical scheme that the device of the utility model intensification separation valence state chromium is taked is:
A kind of intensification separated the device of valence state chromium; be characterized in: device comprises sample load carrier, heating arrangements and inert gas shielding mechanism; the relative sample load carrier of heating arrangements is provided with; directly or indirectly heated sample load carrier, sample load carrier are provided with inert gas shielding mechanism outward, and there is the inert gas blow vent in inert gas shielding mechanism.
The device that the utility model intensification separates valence state chromium can also adopt following technical scheme:
Described intensification separates the device of valence state chromium, and be characterized in: heating arrangements is an electric heater, and the sample load carrier is tungsten or graphite material example boat, and the heating element heater of electric heater directly is assemblied in tungsten or graphite material example boat.
Described intensification separates the device of valence state chromium, is characterized in: the heating element heater of electric heater even is equipped with the heating and temperature control device.
Described intensification separates the device of valence state chromium, and be characterized in: tungsten or graphite material example boat have inert gas shielding mechanism radome, and there is protective cover in the inert gas shielding mechanism radome outside.
Described intensification separates the device of valence state chromium; be characterized in: heating arrangements is outer heater; the sample load carrier is pottery or quartz specimen boat; pottery or quartz specimen boat are positioned at tube furnace; tube furnace is connected with inert gas simultaneously as inert gas shielding mechanism; outer heater heating tube furnace mode is carried out pottery or quartz specimen boat indirect, realizes that the sample intensification separates.
Described intensification separates the device of valence state chromium, and be characterized in: pottery or tube furnace position, quartz specimen boat top are provided with the sample feeding mouth, and the side has through hole to connect argon tanks.
Described intensification separates the device of valence state chromium, and be characterized in: device is provided with sample treatment mechanism, and sample treatment mechanism comprises water-bath or graphite heater, is provided with sample cell in the heater, and sample cell connects syringe pump by probe tube.
Described intensification separates the device of valence state chromium, and be characterized in: sample cell is provided with sample introduction needle, and sample cell is connected syringe pump through sample introduction needle with probe tube.
Advantage and the good effect that the utlity model has are:
Heat up and separate the device of valence state chromium owing to adopted the utility model brand-new technology scheme, compared with prior art, the utlity model has simple in structurely, assembling is compact, easy to operate, economical and practical, versatility is good, applied range, select effective, the separative efficiency height is measured advantages such as accurate, but extensive use is carried out Cr (III) and separated detection with Cr (VI).
Description of drawings
Fig. 1 is the apparatus structure schematic diagram that the direct-heating type intensification separates valence state chromium; 9 is the example boat of tungsten or graphite material among the figure, and sample is dripped thereon, and the energising of this example boat can be heated to different temperatures, with the realization temperature programming; 10 is radome, for sample evaporation provides the environment isolated with ambient atmosphere; 11 is Cr (III) complex compound that steams at a certain temperature; 12 is the electrode to the example boat power supply; Inert gas entrance is arranged, for sample evaporation provides inert gas environment.
Fig. 2 is the apparatus structure schematic diagram that the indirect heating type intensification separates valence state chromium; 21 is pottery or quartz specimen boat among the figure, and sample is dripped thereon; 15 is Cr (III) complex compound that steams at a certain temperature; 16 is tube furnace, with the realization temperature programming; Inert gas entrance is arranged, for sample evaporation provides inert gas environment.
Fig. 3 is a sample pre-treatments apparatus structure schematic diagram; 3 represent heating module among the figure, can be water-bath or graphite heating piece; 4 is sample introduction needle, is used for absorption/filling sample solution; 5 is probe tube, is used to connect sample introduction needle and syringe pump 6, and the sample that syringe pump 6 is drawn is stored in wherein, afterwards again by syringe pump 6 with sample from wherein be filled into example boat (9 or 21); 6 is syringe pump, is used for quantitative absorption/filling sample solution; 2 is the filter washing water inlet, detergent line behind the sample solution that is used to annotate; 1 is sample cell, and sample is given birth to complex reaction at Guan Zhongyu complexing agent hybrid concurrency.
Fig. 4 is the FB(flow block) that Cr (III) separates with Cr (VI).
Among the figure, 1. sample cell, 2. filter washing water inlet, 3. water-bath or graphite heater, 4. sample introduction needle, 5. probe tube, 6. syringe pump, 7. heating and temperature control device, 8. protective cover, 9. example boat, 10. radome, 11. complex compounds, 12. electrode, 13. argon tanks, 14. injection ports, 15. complex compounds, 16. tube furnace, 17. argon tanks, 18. injection ports, 19. outer cover, 20. muffle furnaces, 21. example boats.
The specific embodiment
For further understanding utility model content of the present utility model, characteristics and effect, exemplify following examples now, and conjunction with figs. is described in detail as follows:
Consult accompanying drawing 1, Fig. 2, Fig. 3 and Fig. 4.
Embodiment 1
A kind of intensification separated the device of valence state chromium, comprises sample load carrier, heating arrangements and inert gas shielding mechanism.Heating arrangements is an electric heater, and the sample load carrier is tungsten or graphite material example boat 9, and the heating element heater of electric heater is assemblied in tungsten or graphite material example boat, and tungsten or graphite material example boat are directly heated.The heating element heater of electric heater even is equipped with heating and temperature control device 7.Tungsten or graphite material example boat have inert gas shielding mechanism radome 10, and there is protective cover 8 in the inert gas shielding mechanism radome outside.
The concrete mounting structure and the measuring process thereof of present embodiment:
Sample is added in the sample cell 1, adds complexing agent TTA simultaneously, and the jolting certain hour is realized the complexing of Cr (III) under the heating of heating module; Solution is sucked probe tube 5 by syringe pump 6 afterwards, is filled in the example boat 9 again; Example boat is enclosed in the radome 10 again, argon tanks 13 feeds the argon gas (Ar) of 50 ml/min by inert gas entrance, apply certain voltage, electric current for example boat 9 by heating and temperature control device 7 afterwards, make it temperature and be elevated to the temperature (700 ℃) that Cr (III) complex compound steams, under this temperature, kept 60 seconds, the complex compound 11 of Cr (III) is evaporated fully, and realization Cr (VI) separates with Cr (III's).The volatility of Cr (III) can reach more than 95%, and the retention rate of Cr (VI) reaches more than 98%.
Embodiment 2
A kind of intensification separated the device of valence state chromium, comprises sample load carrier, heating arrangements and inert gas shielding mechanism.Heating arrangements is outer heater muffle furnace 20; the sample load carrier is pottery or quartz specimen boat 21; pottery or quartz specimen boat 21 are positioned at tube furnace 16; tube furnace 16 is connected with inert gas simultaneously as inert gas shielding mechanism; tube furnace is put into muffle furnace 20; carry out pottery or quartz specimen boat indirect, realize that the sample intensification separates.Pottery or tube furnace position, quartz specimen boat 21 top are provided with sample feeding mouth 18, and the side has through hole to connect argon tanks 17.
The concrete mounting structure and the measuring process thereof of present embodiment:
Sample is added in the sample cell 1, adds complexing agent TTA simultaneously, and the jolting certain hour is realized the complexing of Cr (III) under the heating of heating module; Solution is sucked probe tube 5 by syringe pump 6 afterwards, is filled in the example boat 21 again; Again example boat 21 is enclosed in the tube furnace 16, argon tanks 17 feeds the argon gas (Ar) of 50 ml/min by inert gas entrance, give example boat 21 heating by muffle furnace intensification tube furnace afterwards, make it temperature and be elevated to the temperature (600 ℃) that Cr (III) complex compound steams, under this temperature, kept 80 seconds, the complex compound 15 of Cr (III) is evaporated fully, and realization Cr (VI) separates with Cr (III's).The volatility of Cr (III) can reach more than 96%, and the retention rate of Cr (VI) reaches more than 98%.
More than two embodiment heat up and separate the device of valence state chromium, be equipped with sample treatment mechanism, sample treatment mechanism comprises water-bath or graphite heater 3, is provided with sample cell 1 in the heater, sample cell 1 is connected syringe pump 6 through sample introduction needle 4 with probe tube 5.Syringe pump 6 is communicated with filter washing water inlet 2, can realize that pipeline cleans, and guarantees to measure accurately.
Present embodiment can heat up and separate valence state chromium, realizes the purpose of invention, has described advantage and good effect.
Claims (8)
1. one kind heats up and separates the device of valence state chromium; it is characterized in that: device comprises sample load carrier, heating arrangements and inert gas shielding mechanism; the relative sample load carrier of heating arrangements is provided with; directly or indirectly heated sample load carrier, sample load carrier are provided with inert gas shielding mechanism outward, and there is the inert gas blow vent in inert gas shielding mechanism.
2. intensification according to claim 1 separates the device of valence state chromium, and it is characterized in that: heating arrangements is an electric heater, and the sample load carrier is tungsten or graphite material example boat, and the heating element heater of electric heater directly is assemblied in tungsten or graphite material example boat.
3. intensification according to claim 2 separates the device of valence state chromium, it is characterized in that: the heating element heater of electric heater even is equipped with the heating and temperature control device.
4. intensification according to claim 2 separates the device of valence state chromium, and it is characterized in that: tungsten or graphite material example boat have inert gas shielding mechanism radome, and there is protective cover in the inert gas shielding mechanism radome outside.
5. intensification according to claim 1 separates the device of valence state chromium; it is characterized in that: heating arrangements is outer heater; the sample load carrier is pottery or quartz specimen boat; pottery or quartz specimen boat are positioned at tube furnace; tube furnace is connected with inert gas simultaneously as inert gas shielding mechanism; outer heater heating tube furnace mode is carried out pottery or quartz specimen boat indirect, realizes that the sample intensification separates.
6. intensification according to claim 5 separates the device of valence state chromium, and it is characterized in that: pottery or tube furnace position, quartz specimen boat top are provided with the sample feeding mouth, and the side has through hole to connect argon tanks.
7. intensification according to claim 1 separates the device of valence state chromium, and it is characterized in that: device is provided with sample treatment mechanism, and sample treatment mechanism comprises water-bath or graphite heater, is provided with sample cell in the heater, and sample cell connects syringe pump by probe tube.
8. intensification according to claim 1 separates the device of valence state chromium, and it is characterized in that: sample cell is provided with sample introduction needle, and sample cell is connected syringe pump through sample introduction needle with probe tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010202191797U CN201701756U (en) | 2010-06-09 | 2010-06-09 | Device for separating valence chromium by temperature rise |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010202191797U CN201701756U (en) | 2010-06-09 | 2010-06-09 | Device for separating valence chromium by temperature rise |
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| CN201701756U true CN201701756U (en) | 2011-01-12 |
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| CN2010202191797U Expired - Fee Related CN201701756U (en) | 2010-06-09 | 2010-06-09 | Device for separating valence chromium by temperature rise |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984065A (en) * | 2017-03-14 | 2017-07-28 | 中国地质大学（武汉） | A kind of method of scene separation chromium form |
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2010
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984065A (en) * | 2017-03-14 | 2017-07-28 | 中国地质大学（武汉） | A kind of method of scene separation chromium form |
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| 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: 20110112 Termination date: 20110609 |