CN204154649U - A kind of chromium Elemental Speciation Analysis device - Google Patents
A kind of chromium Elemental Speciation Analysis device Download PDFInfo
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- CN204154649U CN204154649U CN201420666418.1U CN201420666418U CN204154649U CN 204154649 U CN204154649 U CN 204154649U CN 201420666418 U CN201420666418 U CN 201420666418U CN 204154649 U CN204154649 U CN 204154649U
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- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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Abstract
The utility model provides a kind of chromium Elemental Speciation Analysis device, comprise flow injection system and liquid cathode glow discharge atomic emission detection system, in the light source generation of liquid cathode glow discharge atomic emission detection system, graphite rod runs through a sidewall of liquid cell form with level is fixed on liquid cell; Sample injection unit comprises the sample feeding pipe of the bottom of vertical through graphite rod and liquid cell, and the top of sample feeding pipe is positioned at immediately below metal anode, and sample injection unit makes solution to be measured overflow from the top of sample feeding pipe, and forms glow discharge region between metal anode; Flow injection system is connected with sample injection unit to supply solution to be measured, flow injection system comprise there is different valve position sampling valve, for eluent and liquid to be measured being directed into respectively the first peristaltic pump of sampling valve and the second peristaltic pump and being filled with the solid-phase extracting disk of extractant; Solid-phase extracting disk is connected in the different sample introduction positions of sampling valve.
Description
Technical field
The utility model belongs to atomic spectroscopic analysis field, is specifically related to a kind of chromium Elemental Speciation Analysis device.
Background technology
At occurring in nature, the main existence form of chromium (Cr) is Cr (III) and Cr (VI).Wherein, Cr (III) is one of necessary trace element of the mankind, and its major function regulates metabolism, metabolism of blood glucose, and with the synthesis of nucleic acid, ester class and cholesterol, and amino acid whose utilization is relevant, be used to prevent and treat diabetes, hypertension and cancer.But, there were significant differences for the chemical property of Cr (VI) and toxic level and Cr (III), Cr (VI) can destroy the ultrastructure in vegetable cell, suppress growth and development of plants and photosynthesis, and it has stronger DNA damage capability, cytotoxicity and biological accumulation, its compound also can cause various types of gene mutation.Long Term Contact Cr (VI) compound, also can cause allergic and ulcer.Therefore, in environment, the chemical speciation of chromium is most important.
At present, the method both at home and abroad for chromium morphological analysis is mainly some coupling techniques, and these technology mainly first make the different valence state pre-separation of chromium by isolation technics, then use atomic spectrum (mass spectrum) to measure as testing tool.Conventional analytical approach has Solid-Phase Extraction coupling atomic absorption spectrography (AAS), Solid-Phase Extraction coupling inductively coupled plasma spectrometry method, high performance liquid chromatography coupling inductively coupled plasma mass spectrometry etc.Although the detection sensitivity of these coupling techniques is high, detection limit is low, accuracy is high, there is apparatus expensive, operating cost is high, often need the deficiencies such as assist gas, high vacuum environment, high power and elevated operating temperature.
But liquid cathode glow discharge atomic emission spectrum (Solution Cathode Glow Discharge-Atomic Emission Spectroscopy, SCGD-AES) has can under atmospheric pressure direct control, does not need working gas; Instrument power requirement is low, and operating power is less than 100W; Sample feeding is without the need to using the outstanding advantages such as atomizer.But the microplasma temperature produced due to SCGD-AES is lower, and more weak to exciting of chromium, therefore, it only has 200 μ gL to the detection limit of Cr
-1.Researchist improved the sensitivity of SCGD-AES to Cr by interpolation surfactant formic acid and hexadecyltrimethylammonium chloride afterwards, and detection limit is reduced to 65 μ gL
-1with 42 μ gL
-1.But compared with other detecting device, SCGD-AES still can not meet normal demand to the detection limit of Cr, remains blank out to the Determination of Different Valence States of Cr simultaneously.
Solid-Phase Extraction is a kind of straightforward procedure improving instrumental sensitivity, and wherein, solid extracting agent plays vital effect to the raising of the adsorbance of Cr to instrumental sensitivity.The solid extracting agent in the past adopted is organic resin, and they are very limited to the adsorbance of Cr usually, thus limits the raising of sensitivity and enrichment times.
But mesoporous material is easy to carry out the advantages such as chemical modification with the pore passage structure of its larger specific surface area, single pore diameter distribution, high-sequential, adjustable pore size and surface, has been used successfully to separation and the enrichment of heavy metal ion.After adopting two steps, grafting prepares lysine modified SBA-15, applies for patent of invention, and the patent No. is: 2013107390723, and it reaches 76 mgg to the saturated extent of adsorption of Cr (VI)
-1, when pH=5, it not only has quick adsorption performance to Cr (VI) simultaneously, and to Cr (III) not absorption, therefore may be used for the Determination of Different Valence States of Cr.
Utility model content
The utility model is intended to overcome existing high for chromium Valence Analysis apparatus expensive/operating cost, the detection sensitivity of liquid cathode glow discharge atomic emission spectrum to chromium is low waits not enough defect, and the utility model provides a kind of low cost, uses the chromium Elemental Speciation Analysis device of simple, high enrichment times.
The utility model provides a kind of chromium Elemental Speciation Analysis device, comprise flow injection system and liquid cathode glow discharge atomic emission detection system, wherein, the spectrophotometric unit that described liquid cathode glow discharge atomic emission detection system comprises the light source generation producing glow discharge, the grow discharge optical emission spectrometry produced described light source generation carries out light-splitting processing, the detecting unit that the emission spectrum after light-splitting processing is detected and the data processing unit to the data analysis process that described detecting unit produces; Described light source generation comprises the metal anode be connected with the positive pole of high-voltage power supply, the graphite rod, liquid cell and the sample injection unit that are connected with the negative pole of described high-voltage power supply; Described graphite rod runs through a sidewall of described liquid cell form with level is fixed on described liquid cell; Described sample injection unit comprises the sample feeding pipe of the bottom of vertical through described graphite rod and described liquid cell, the top of described sample feeding pipe is positioned at immediately below described metal anode, described sample injection unit makes solution to be measured overflow from the top of described sample feeding pipe, and forms glow discharge region between described metal anode; Described flow injection system is connected to supply solution to be measured with described sample injection unit, described flow injection system comprise there is different valve position sampling valve, for eluent and liquid to be measured being directed into respectively the first peristaltic pump of described sampling valve and the second peristaltic pump and being filled with the solid-phase extracting disk of extractant; Described solid-phase extracting disk is connected in the different sample introduction positions of described sampling valve.
Chromium Elemental Speciation Analysis device of the present utility model, adopt flow injection system and the coupling of liquid cathode glow discharge atomic emission detection system, the analytic process that this device carries out comprises separation and concentration, wash-out and cleaning, by being filled with the solid-phase extracting disk of extractant, the different shape of chromium element can be made to be separated, to achieve effective separation of different shape chromium.Simultaneously by after separation and concentration, reduce liquid cathode glow discharge atomic emission spectrum to the detection limit of chromium, improve mensuration sensitivity.
Preferably, in the utility model, described extractant is lysine modified SBA-15.
According to the utility model, lysine modified SBA-15 has fast selective absorption property to sexavalent chrome, substantially increases the enrichment times of analytical approach, improves and measures sensitivity, reduce the detection limit of SCGD-AES to Cr.
Preferably, in the utility model, described sample injection unit also comprises the 3rd peristaltic pump be connected between described flow injection system and described sample feeding pipe.
According to the utility model, adopt this peristaltic pump to drive described sample feeding pipe sample introduction.This peristaltic pump is common lab peristaltic pump, has fast pumping function key.
Preferably, in the utility model, described light source generation also comprises the three-dimensional platform for installing described liquid cell and described metal anode, and described three-dimensional platform is configured to the position that can regulate described liquid cell and described metal anode in X, Y, Z-direction.
According to the utility model, the position of described liquid cell and described metal anode can be regulated, like this can fine adjustment liquid cell and the metal anode position of going up in any direction.Adjusting position is then detect to allow the light source of plasma fully enter spectrometer.
Preferably, in the utility model, between the positive pole of described high-voltage power supply and described metal anode, be provided with resistance.
According to the utility model, arranging resistance is in order to protection power source, and steady current.
Preferably, in the utility model, described high-voltage power supply can provide the voltage of 0-2000V, the rated current of 0-0.1A; And described resistance is 1 K Ω-1.2 K Ω.
According to the utility model, the setting of above-mentioned voltage, electric current, resistance value is to enable liquid cathode stably produce plasma, ensures the stable of whole circuit simultaneously.
Preferably, in the utility model, described metal anode is diameter is 2 ~ 4mm, and tip is formed as tungsten electrode that diameter is the circle of 1mm or Ti electrode; Described sample feeding pipe is internal diameter is 0.38 mm, and external diameter is the glass capillary of 1.1 mm.
According to the utility model, arranging above-mentioned metal anode is to produce plasma, and arrange above-mentioned sample feeding pipe be in order to make liquid flow into thus produce plasma.
Preferably, in the utility model, described light source generation also comprises the discharging tube be communicated with the bottom of described liquid cell.
According to the utility model, the liquid exceeding regulation liquid level can be discharged from liquid cell by this discharging tube.
Preferably, in the utility model, described eluent is the ammonia spirit of 0.09-0.11mol/L.
According to the utility model, the Cr be adsorbed on above mesoporous material (VI) can elute by this ammoniacal liquor.
Preferably, in the utility model, also comprise and be connected to described flow injection system and the direct three-way connector of described sample injection unit.
According to the utility model, before eluant, eluent enters liquid cathode glow discharge atomic emission spectrum, three-way connector need be added and import the nitric acid liquid as a supplement that concentration is 7%-8%, regulate eluant, eluent pH to be 1, thus ensure stable ignition.
The beneficial effects of the utility model:
Adopt flow injection Solid-Phase Extraction-liquid cathode glow discharge Atomic Emission Spectral Analysis device, make the different shape separation and concentration of chromium element, achieve effective separation of different shape chromium; Have employed novel lysine modified SBA-15 as solid extracting agent, substantially increase the enrichment times of analytical approach, improve and measure sensitivity, reduce detection limit (the 0.75 μ gL of SCGD-AES to Cr
-1); In addition, the utility model square law device price is low, simple to operate, enrichment times is high, good separating effect, is convenient to realize field monitoring, and this detects lay a good foundation to realizing the online of chromium and field.
Accompanying drawing explanation
Fig. 1 shows the schematic diagram of the chromium Elemental Speciation Analysis device in an embodiment of the present utility model;
Fig. 2 shows the valve position conversion schematic diagram of the sampling valve of the flow injection system in an embodiment of the present utility model.
Embodiment
Below some exemplary embodiments are listed further better the utility model to be described.Should understand; the above-mentioned embodiment that the utility model describes in detail; and following examples are only not used in restriction scope of the present utility model for illustration of the utility model, some nonessential improvement that those skilled in the art makes according to foregoing of the present utility model and adjustment all belong to protection domain of the present utility model.In addition, concrete proportioning, time, temperature etc. in following technological parameter are also only exemplary, and those skilled in the art can select suitable value in the scope of above-mentioned restriction.
The utility model provides a kind of chromium Elemental Speciation Analysis device, and mainly comprise flow injection system and liquid cathode glow discharge atomic emission detection system, analytic process comprises separation and concentration, wash-out and cleaning.Wherein, principle in separation and concentration process is that the mesoporous material in solid-phase extracting disk only has absorption to Cr (VI), to Cr (III) not absorption, therefore when the solution containing Cr (VI) and Cr (III) is by mesoporous material, Cr (VI) can be adsorbed onto above material and form enrichment, but Cr (III) can flow out material with solution thus form separation, the effect of separation and concentration is separated with Cr (III) by Cr (VI), carries out enrichment to Cr (VI) simultaneously.The principle of wash-out is that the Cr be enriched on mesoporous material (VI) can elute by ammoniacal liquor, effect passes into certain density ammoniacal liquor to be eluted above mesoporous material by Cr (VI), then pass into liquid cathode glow discharge atomic emission spectrum and detect.The principle of cleaning goes after wash-out to have remaining ammoniacal liquor in pipeline and phase extracting disk, if directly pass into acid testing liquid can affect its acidity, thus cause the adsorption efficiency of mesoporous material to Cr (VI) to change causing test result inaccurate, so must clean pipeline with deionized water, effect removes remaining ammoniacal liquor.This analysis device improves liquid cathode glow discharge atomic emission spectrum to the sensitivity of chromium, reduces the detection limit of chromium, meanwhile, the chromium of different shape is separated effectively.
Liquid cathode glow discharge atomic emission detection system about using in the utility model:
This liquid cathode glow discharge atomic emission detection system applies for patent of invention, and this patent publication No. is CN103163116 A, simply illustrates below to this detection system.This liquid cathode glow discharge atomic emission detection system comprises light source and occurs, beam splitting system, pick-up unit, data handling system four parts, described light source generating portion comprises high-voltage power supply, resistance 10, three-dimensional platform, metal anode 9, peristaltic pump 6, liquid cell 11, sample feeding pipe 13(containing glass capillary) and discharging tube 14.Sample solution sample introduction is introduced through peristaltic pump 6.Liquid cell 11 and metal anode 9 are installed on X, Y, three-dimensional platform that Z-direction is adjustable.Sample feeding pipe 13 is connected with liquid cell with discharging tube 14 passing hole channel.
In an embodiment of the present utility model, described high-voltage power supply can provide 0 ~ 2000 V high pressure, and rated current is 0.1 A; Resistance 10 can be 1 K Ω or 1.2 K Ω etc.
In an embodiment of the present utility model, described metal anode material 9 is tungsten or Ti electrode, and diameter is 2 ~ 4 mm, and its tip is circular, and diameter is 1 mm; Sample feeding pipe 13 uses glass capillary, and internal diameter is 0.38 mm, and external diameter is 1.1 mm; Discharging tube 14 internal diameter 2 mm, external diameter is 4 mm; Designed liquid cell 11 is made up through certain processes of polytetrafluoroethylmaterial material.
High-voltage power supply positive pole wire is out connected with metal anode 9 through resistance 10; Negative pole is then connected with graphite electrode 7, and graphite electrode 7 is horizontally fixed on the side of liquid cell 11 wall.Sample feeding pipe is fixed in the pore on graphite rod 7, and discharging tube 14 is inserted in the corresponding pore of liquid cell.
Liquid cell 11 and metal anode 9 are installed on X, Y, three-dimensional platform that Z-direction is adjustable; Three-dimensional platform both can realize coarse adjustment also can realize fine setting.
Liquid cathode glow discharge atomic emission spectrum experimental provision igniting need pH be 1 electrolytic solution (such as nitric acid).
Peristaltic pump 6 is common lab peristaltic pump, has fast pumping function key.
Graphite rod 7 level runs through liquid cell 11 wall and is fixed on the side of liquid cell 11; Sample injection unit comprises vertical through described liquid cell 11 and top is positioned at sample feeding pipe 13 immediately below described metal anode 9, and meanwhile, sample feeding pipe 13 vertically runs through the graphite rod 7 of horizontal positioned; Sample injection unit makes solution to be measured overflow from the top of sample feeding pipe 13, forms glow discharge region 8 between the solution to be measured that sample feeding pipe 13 top is overflowed and metal anode 9.The sample of liquid cathode glow discharge atomic emission spectrum adopts peristaltic pump to drive sample feeding pipe sample introduction.SCGD-AES specific features described in the utility model is the nitric acid (it produces stable plasma, produces maximum signal simultaneously) of the electrolytic solution employing pH=1 in liquid cell 11, and keeping at a distance in the top of sample feeding pipe 13 and metal anode 9 tip is 3 mm.At ambient pressure, be a pole with solution, tungsten or Ti electrode are anode, by applying high pressure to two electrodes, thus cause interelectrode gas generation electric discharge to produce; The region of glow discharge namely between metal anode 9 and the sample solution of glass capillary 13 tip spilling produces.The emission spectrum that region of discharge 8 produces focuses on through lens 15 and arrives monochromator, is then obtained the spectral intensity of respective element by the detection of photomultiplier (PMT), thus quantitative test constituent content wherein.
Because line strength of atomic emission spectrum is directly proportional to the concentration of component tested in sample, therefore quantitative test can be carried out to element.In mensuration process, mainly carried out the mensuration of element-intensities by a SpectraSense software, in mensuration process, be divided into chosen elements characteristic spectral line, drawing standard curve, mensuration.The characteristic spectral line that we select is 357.9nm, and standard solution, as standard solution, first measures, its intensity and concentration drawn a typical curve by the Cr (VI) of configuration variable concentrations.Finally, will the solution measured be needed to measure, the relation of using degree and concentration calculates the concentration of solution.
About the flow injection system used in the utility model (flow injection instruments)
Flow injection instruments comprises 2 peristaltic pumps 4a, 4b as power unit and a transposition valve (i.e. sampling valve) 5, and solid-phase extracting disk 12 is connected between the different sample introduction positions of transposition valve 5.
In an embodiment of the present utility model, eluant, eluent is the ammoniacal liquor of 0.1mol/L, and the flow velocity of eluant, eluent is 1.5mL/min, and elution time is 120s; Enrichment rate is 4mL/min, and enrichment time is 420s; Washed with de-ionized water speed is 4 mL/min, and scavenging period is 60s.In peristaltic pump, flow rate of liquid is 2 mL/min.
Before eluant, eluent enters liquid cathode glow discharge atomic emission spectrum combined system, import the nitric acid liquid as a supplement that concentration is 7%-8%, regulate eluant, eluent pH to be 1, thus ensure stable ignition.In an embodiment of the present utility model, the flow velocity of replenisher is 0.5 mL/min.
Solid-phase extracting disk 12 described in the utility model is commercial prod, cheap, without the need to special customization.In an embodiment of the present utility model, the commercial filtration head that what solid-phase extracting disk 12 adopted is external diameter is 2.5 centimetres, internal diameter is 0.22 micron.
The solid extracting agent of filling in solid-phase extracting disk 12 is that lysine modified SBA-15(applies for patent of invention, and the patent No. is: 2013107390723).In an embodiment of the present utility model, sorbent material loading described in the utility model is 25-35 mg.
In flowing injection device, comprise peristaltic pump 4a, a peristaltic pump 4b and sampling valve 5.Described sampling valve 5 is divided into Fil and Inj two valve position, and sample introduction position corresponding in each valve position communicates.Fig. 2 is the valve position conversion schematic diagram of flow injection sampling valve of the present utility model.Visible in Fig. 2 in Inj valve position, eluant, eluent pipeline connecting mode is: from sample introduction position 1-1 to 1-2, then uses tubes connection sample introduction position 3-2, flows into detecting device (liquid cathode glow discharge atomic emission spectrum combined system) from 3-1; Liquid pipeline connected mode to be measured is: from sample introduction position 2-1 to 2-2, then access 4-2 with after tubes connection solid-phase extracting disk, flows into waste liquid pool from 4-1.In Fil valve position, eluant, eluent pipeline connecting mode is: from 1-1 to 2-2, then flows into 4-2 through solid-phase extracting disk, flows into detecting device from 3-1; Liquid to be measured stops flowing.
In the utility model, the using method of chromium Elemental Speciation Analysis device is:
In separation and concentration part, the valve position of flow injection is Inj, and testing liquid first enters solid-phase extracting disk by peristaltic pump 4b from 2-1 and the 2-2 sample introduction position of flow injection, then enters waste liquid bottle from 4-2 and 4-1 sample introduction position; Eluent enters flow injection by peristaltic pump 4a from 1-1 and 1-2 sample introduction position, then enters detection system from 3-2 and 3-1 sample introduction bit stream.Now, in order to the igniting meeting liquid cathode glow discharge atomic emission spectrum requires---solution acidity, near pH=1, before entering detection system, must import the acidity that replenisher changes tracer liquid.Then, by peristaltic pump (c) 6, tracer liquid is passed into SCGD-AES to detect.At elution fraction, it is Fil that the sampling valve of flow injection changes valve position, and testing liquid stops flowing, and eluent enters solid-phase extracting disk from 1-1 and 2-2 sample introduction position, eluted by the Cr be enriched in adsorbent (VI), eluent enters detection system from 4-2 and 3-1 sample introduction position again.At cleaning part, the valve position of flow injection is adjusted to Inj, changes liquid to be measured into washed with de-ionized water pipeline, all the other steps are identical with separation and concentration part.
In concrete form analytic process, first configure the Cr (VI) of two bottles of same concentrations and the solution of Cr (III), wherein will use H by one bottle of solution
2o
2cr (III) is completely oxidized to Cr (VI), respectively these two bottles of solution are passed into the content that this device measures Cr (VI), the content of Cr (III) is the difference of the content of Cr (VI) in the content of total Cr and original solution.Effect in separation and concentration process is separated with Cr (III) by Cr (VI), carries out enrichment to Cr (VI) simultaneously.The effect of wash-out passes into certain density ammoniacal liquor to be eluted above mesoporous material by Cr (VI), then pass into liquid cathode glow discharge atomic emission spectrum and detect.Remaining ammoniacal liquor is removed in the effect of cleaning.
The beneficial effects of the utility model are: 1. adopt flow injection Solid-Phase Extraction-liquid cathode glow discharge Atomic Emission Spectral Analysis device, make the different shape separation and concentration of chromium element, achieve effective separation of different shape chromium; 2. have employed novel lysine modified SBA-15 as solid extracting agent, substantially increase the enrichment times of analytical approach, improve and measure sensitivity, reduce detection limit (the 0.75 μ gL of SCGD-AES to Cr
-1);
The utility model is the chromium Elemental Speciation Analysis device and analytical approach thereof that use in a kind of analytical chemistry field, by flow injection instruments and the coupling of liquid cathode glow discharge atomic emission spectrum, solid-phase extracting disk is connected in described flow injection instruments, that solid extracting agent adopts is novel lysine modified SBA-15, it has fast selective absorption property to sexavalent chrome, the different shape of chromium element is separated, achieves effective separation of different shape chromium.Simultaneously by after separation and concentration, reduce liquid cathode glow discharge atomic emission spectrum to the detection limit of chromium, improve mensuration sensitivity;
In addition, the utility model square law device price is low, simple to operate, enrichment times is high, good separating effect, is convenient to realize field monitoring, and this detects lay a good foundation to realizing the online of chromium and field.
Embodiment
Containing 100 μ gL
-1cr (III) and 40 μ gL
-1the sewage solution of Cr (VI) is (containing Ca, Mg, Na, SO in sewage
4 2-with K etc.) 2-1 and the 2-2 sample introduction position of Inj valve position is flowed through from peristaltic pump 4b, flow into solid-phase extracting disk enrichment 420s, flow out from sample introduction position 4-2 and 4-1 and enter waste liquid bottle, now, the ammoniacal liquor of 0.1mol/L flows through 1-1 and the 1-2 sample introduction position of Inj valve position from peristaltic pump 4a with the speed of 1.5mL/min, by tubes connection to 3-2 and 3-1 sample introduction position, flow into peristaltic pump c, the nitric acid of 7.5% as a supplement liquid together flows into peristaltic pump (c) 6 by threeway and eluent, peristaltic pump (c) 6 enters SCGD-AES with the speed of 2mL/min, when after bubble collapse in conduit, 1100V high direct voltage is loaded between glass capillary and tungsten electrode 9, then the fast pump key in peristaltic pump (c) 6 is pressed, flow velocity increases, observe in region of discharge 8 plasma light stable after, recover former flow velocity.After enrichment, the valve position of flow injection is converted to Fil, and now, liquid to be measured stops flowing; The ammoniacal liquor of 0.1mol/L flows through 1-1 and the 2-2 sample introduction position of Fil valve position from peristaltic pump 4a with the speed of 1.5mL/min, flow into solid-phase extracting disk by after Cr (VI) wash-out after enrichment, peristaltic pump (c) 6 is flowed into through sample introduction position 4-2 and 3-1, the nitric acid of 7%-8% as a supplement liquid imports eluent and together flows into peristaltic pump (c) 6, and peristaltic pump (c) 6 enters SCGD-AES with the speed of 2mL/min and detects.After wash-out 200s, flow injection is converted to Inj valve position, and deionized water flows through 2-1 and the 2-2 sample introduction position of Inj valve position from peristaltic pump 4b, flows into solid-phase extracting disk cleaning 60s, flows out enter waste liquid bottle from sample introduction position 4-2 and 4-1.
Then, will containing 100 μ gL
-1cr (III) and 40 μ gL
-1after the surplus solution hydrogen peroxide oxidation of Cr (VI), carry out the operation of same step, test result is the content of total chromium in solution.Three times test result is as shown in table 1.The content of display Cr (VI) is 39.5 ± 1.2 μ gL
-1, the content of Cr (III) is 101.2 ± 1.4 μ gL
-1, the recovery of Cr (VI) is 99%, can the different valence state of separation of C r effectively.
Table 1:
Claims (10)
1. a chromium Elemental Speciation Analysis device, is characterized in that, described chromium Elemental Speciation Analysis device comprises flow injection system and liquid cathode light electric discharge atomic emission detection system, wherein,
The spectrophotometric unit that described liquid cathode glow discharge atomic emission detection system comprises the light source generation producing glow discharge, the grow discharge optical emission spectrometry produced described light source generation carries out light-splitting processing, the detecting unit that the emission spectrum after light-splitting processing is detected and the data processing unit to the data analysis process that described detecting unit produces;
Described light source generation comprises the metal anode be connected with the positive pole of high-voltage power supply, the graphite rod, liquid cell and the sample injection unit that are connected with the negative pole of described high-voltage power supply;
Described graphite rod runs through a sidewall of described liquid cell form with level is fixed on described liquid cell;
Described sample injection unit comprises the sample feeding pipe of the bottom of vertical through described graphite rod and described liquid cell, the top of described sample feeding pipe is positioned at immediately below described metal anode, described sample injection unit makes solution to be measured overflow from the top of described sample feeding pipe, and forms glow discharge region between described metal anode;
Described flow injection system is connected to supply solution to be measured with described sample injection unit, described flow injection system comprise there is different valve position sampling valve, for eluent and liquid to be measured being directed into respectively the first peristaltic pump of described sampling valve and the second peristaltic pump and being filled with the solid-phase extracting disk of extractant;
Described solid-phase extracting disk is connected in the different sample introduction positions of described sampling valve.
2. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, described extractant is lysine modified SBA-15.
3. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, described sample injection unit also comprises the 3rd peristaltic pump be connected between described flow injection system and described sample feeding pipe.
4. chromium Elemental Speciation Analysis device according to claim 1, it is characterized in that, described light source generation also comprises the three-dimensional platform for installing described liquid cell and described metal anode, and described three-dimensional platform is configured to the position that can regulate described liquid cell and described metal anode in X, Y, Z-direction.
5. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, is provided with resistance between the positive pole of described high-voltage power supply and described metal anode.
6. chromium Elemental Speciation Analysis device according to claim 5, is characterized in that, described high-voltage power supply can provide the voltage of 0-2000V, the rated current of 0-0.1A; And described resistance is 1 K Ω-1.2 K Ω.
7. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, described metal anode is diameter is 2 ~ 4mm, and tip is formed as tungsten electrode that diameter is the circle of 1mm or Ti electrode; Described sample feeding pipe is internal diameter is 0.38 mm, and external diameter is the glass capillary of 1.1 mm.
8. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, described light source generation also comprises the discharging tube be communicated with the bottom of described liquid cell.
9. chromium Elemental Speciation Analysis device according to claim 1, is characterized in that, described eluent is the ammonia spirit of 0.09-0.11mol/L.
10., according to described chromium Elemental Speciation Analysis device arbitrary in claim 1-9, it is characterized in that, also comprise the three-way connector be connected between described flow injection system and described sample injection unit.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104964965A (en) * | 2015-05-28 | 2015-10-07 | 国家地质实验测试中心 | Portable liquid cathode glow discharge element analyzer |
| CN105651760A (en) * | 2015-12-31 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Microplasma apparatus suitable for metallic element analysis in gas |
| CN105842230A (en) * | 2016-03-29 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Device and method for the detection of heavy metal elements |
| CN106568833A (en) * | 2016-10-11 | 2017-04-19 | 中国科学院上海硅酸盐研究所 | Photochemical steam generator and liquid cathode glow discharge spectrometer coupled analysis apparatus and method for detecting heavy metal by using apparatus |
| CN107271425A (en) * | 2017-05-12 | 2017-10-20 | 中国科学院上海硅酸盐研究所 | A kind of instantaneous sample introduction liquid cathode glow discharge Atomic Emission Spectral Analysis device of suspension and its analysis method |
| WO2019068191A1 (en) * | 2017-10-03 | 2019-04-11 | Innotech Alberta Inc. | Reduction of molecular background emission and sample matrix management in a solution cathode glow discharge |
| CN110658182A (en) * | 2018-06-28 | 2020-01-07 | 中国科学院上海硅酸盐研究所 | Portable metal ion water quality analyzer and detection method thereof |
| US10705023B2 (en) | 2015-12-31 | 2020-07-07 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Solution cathode glow discharge plasma-atomic emission spectrum apparatus and method capable of performing direct gas sample introduction and used for detecting heavy metal element |
| CN111935894A (en) * | 2019-05-13 | 2020-11-13 | 中国科学院上海硅酸盐研究所 | Atmospheric pressure liquid anode glow discharge plasma device |
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| CN104964965A (en) * | 2015-05-28 | 2015-10-07 | 国家地质实验测试中心 | Portable liquid cathode glow discharge element analyzer |
| CN105651760A (en) * | 2015-12-31 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Microplasma apparatus suitable for metallic element analysis in gas |
| US10705023B2 (en) | 2015-12-31 | 2020-07-07 | Shanghai Institute Of Ceramics, Chinese Academy Of Sciences | Solution cathode glow discharge plasma-atomic emission spectrum apparatus and method capable of performing direct gas sample introduction and used for detecting heavy metal element |
| CN105651760B (en) * | 2015-12-31 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | A kind of microplasma device of the metallic element analysis suitable for gas |
| CN105842230B (en) * | 2016-03-29 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | A kind of device and method for heavy metal element detection |
| CN105842230A (en) * | 2016-03-29 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Device and method for the detection of heavy metal elements |
| CN106568833A (en) * | 2016-10-11 | 2017-04-19 | 中国科学院上海硅酸盐研究所 | Photochemical steam generator and liquid cathode glow discharge spectrometer coupled analysis apparatus and method for detecting heavy metal by using apparatus |
| CN106568833B (en) * | 2016-10-11 | 2019-04-16 | 中国科学院上海硅酸盐研究所 | A kind of liquid cathode glow discharge optical emission spectrometry device and method for heavy metal analysis |
| CN107271425A (en) * | 2017-05-12 | 2017-10-20 | 中国科学院上海硅酸盐研究所 | A kind of instantaneous sample introduction liquid cathode glow discharge Atomic Emission Spectral Analysis device of suspension and its analysis method |
| WO2019068191A1 (en) * | 2017-10-03 | 2019-04-11 | Innotech Alberta Inc. | Reduction of molecular background emission and sample matrix management in a solution cathode glow discharge |
| US10962483B2 (en) | 2017-10-03 | 2021-03-30 | Innotech Alberta Inc. | Reduction of molecular background emission and sample matrix management in a solution cathode glow discharge |
| CN110658182A (en) * | 2018-06-28 | 2020-01-07 | 中国科学院上海硅酸盐研究所 | Portable metal ion water quality analyzer and detection method thereof |
| CN111935894A (en) * | 2019-05-13 | 2020-11-13 | 中国科学院上海硅酸盐研究所 | Atmospheric pressure liquid anode glow discharge plasma device |
| CN112858259A (en) * | 2019-11-26 | 2021-05-28 | 中国科学院上海硅酸盐研究所 | Hydride generation-atmospheric pressure liquid anode glow discharge atomic spectrum device |
| CN112461814A (en) * | 2020-11-24 | 2021-03-09 | 北京市理化分析测试中心 | On-line detection device and detection method for thallium in water |
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