CN207379929U - A kind of novel portable liquid cathode glow discharge spectrometry - Google Patents

A kind of novel portable liquid cathode glow discharge spectrometry Download PDF

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Publication number
CN207379929U
CN207379929U CN201721567368.1U CN201721567368U CN207379929U CN 207379929 U CN207379929 U CN 207379929U CN 201721567368 U CN201721567368 U CN 201721567368U CN 207379929 U CN207379929 U CN 207379929U
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China
Prior art keywords
glow discharge
cathode glow
liquid cathode
novel portable
portable liquid
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Expired - Fee Related
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CN201721567368.1U
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Chinese (zh)
Inventor
袁继海
詹秀春
刘晓
石云峰
樊兴涛
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STATE GEOLOGY EXPERIMENT AND TEST CENTER
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STATE GEOLOGY EXPERIMENT AND TEST CENTER
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems 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
    • G01N21/69Systems 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 specially adapted for fluids, e.g. molten metal
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66Systems 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
    • G01N21/67Systems 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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  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The utility model is related to spectrum analysis fields, are specifically a kind of novel portable liquid cathode glow discharge spectrometry, and electric installation, CCD spectrometers and data handling system are supplied including gravity flow sampling structure, embedded liquid cathode glow discharge structure, solar panels;The gravity flow sampling device does stent by a telescopic rod, and cantilever tip has hook, and hook is used for placing sample solution bottle;Sample solution bottom of bottle portion connects one end of sample introduction hose, and the other end of sample introduction hose connects embedded liquid cathode glow discharge structure;The cathode of the embedded liquid cathode glow discharge structure is taper graphite, and anode is tungsten filament, and fills optical filter and focus on light microscopic;The focusing light microscopic connects CCD spectrometers by optical fiber, and CCD spectrometers are connected with data handling system;Each instrument provides electric energy by solar panels for electric installation.The portable fluid cathode glow discharging spectrometer so designed is small, light-weight, easy to carry, the field in-situ analysis available for elements such as Li, K in water body.

Description

A kind of novel portable liquid cathode glow discharge spectrometry
Technical field
The utility model is related to spectrum analysis fields, and in particular to a kind of novel portable liquid based on CCD detector Cathode glow discharging spectrometer.
Background technology
Lithium is the ideal material of new century green energy resource (such as lithium battery) and alloy in lightweight, has the title of " energy upstart ", is A kind of important strategic resource and various countries is subject to increasingly to pay attention to.China is the country that saline lake lithium resource is most abundant in the world One, the lithium resource reserves whole world is number three, but has been verified the 87% of lithium resource and all contained in salt lake bittern, is mainly distributed on west The western remote districts such as Tibetan and Qinghai, sample are transported to the substantial amounts of human and material resources of laboratory test needs and financial support, can not Analysis result is provided in time, thus is badly in need of researching and developing a kind of minimizing, is portable, is easy to operate, analyzing speed for suitable field assay Degree is fast, the reliable novel instrument of analysis result.
The common inductively coupled plasma atomic emission in laboratory (ICP-AES), inductivity coupled plasma mass spectrometry (ICP-MS), the large-scale instruments such as atomic absorption spectrum (FAAS), Flame atomic emission spectrophotometry (FAES) be required for carrier gas, combustion gas or The flow conditions such as combustion-supporting gas can not minimize equipment instrument, and gravimetric method, volumetric method, ion color in traditional analysis Spectrometry, electrochemical method etc. because it is cumbersome, pretreatment process is complicated, measure the cycle it is long, can not realize field quick analysis Target.Field in-situ analysis is using more portable energy Dispersive-X-Ray Fluorescence spectroscopic methodology (ED-XRF) because by principle of instrument Limitation, analyzable element species are limited, can not also analyze light element such as Li.Start from the liquid to grow up the nineties in last century Body cathode glow discharging spectrometer can be run under atmospheric pressure environment, and without carrier gas and vacuum environment, atomising device is not required, can More than 20 are measured simultaneously and plants metallic element, can also measure light element Li, are a kind of potential available for the new of field in-situ analysis Instrument.
At present, based on atmospheric pressure liquid cathode glow discharge device it is essentially all and inductively-coupled plasma spectrometer It is combined, detection device is made of monochromator and photoelectric multiplier, and equipment instrument is larger, does not meet field in-situ analysis to instrument The miniaturization of body product, the requirement of portability, need to carry out miniaturization transformation to instrument.Meanwhile traditional peristaltic pump input mode It is unfavorable for field in-situ analysis, it is anxious to design a kind of new input mode to improve instrument work efficiency.Finally, generator etc. is carried Power supply unit can increase the burden of field analysis personnel, be badly in need of being transformed field assay instrument for electric installation.These into The technical issues that need to address are developed for field in-situ analysis portable instrument.
Utility model content
For the deficiency of present technology, the purpose of this utility model is to provide a kind of for the portable of field in-situ analysis Formula liquid cathode glow discharge spectrometry, for metal cations such as Li, K in the water bodys such as the western salt lake bittern from far-off regions in China Quick analysis.
To achieve these goals, a kind of novel portable liquid cathode glow discharge optical emission spectrometry provided by the utility model Instrument, including sampling structure and for electric installation, wherein, the sampling structure be gravity flow sampling structure, the gravity flow sampling structure Include stent, sample solution bottle and a sample introduction hose of the telescopic and top with hook again;The sample solution bottle is hung It puts on the hook of cantilever tip, the bottom of the sample solution bottle is fixedly connected with one end of sample introduction hose, and the sample introduction hose It is connected with the inner cavity of above-mentioned sample solution bottle;The other end of the sample introduction hose connects embedded liquid cathode glow discharge structure In cathode;The embedded liquid cathode glow discharge structure is connected with current-voltage regulator and display by conducting wire, The current-voltage regulator is connected by conducting wire with constant current constant voltage dual pressure controller, and the constant current constant voltage dual pressure controller is by leading Line is connected with the anode in embedded liquid cathode glow discharge structure and cathode;The bottom of the cathode passes through conduit and waste liquid Bottle connection;Aperture is provided on the outer cover of the embedded liquid cathode glow discharge structure, installs and filters in aperture external application stent Piece and focusing transmissive mirror, focus on transmissive mirror and are connected by optical fiber with CCD detector;The CCD detector passes through data cable and number It is connected according to processing system;It is described to include folding solar charger, the folding solar charger and phosphorus again for electric installation Sour lithium iron battery group is connected by conducting wire.
The utility model has abandoned the design for traditionally using peristaltic pump input mode, and uses gravity flow input mode instead, In suitable height, solution can fully rely on gravity sample introduction.Solution continuously flows into the cathode in cathode glow discharging area, point Fire is stablized, and signal is steady, is conducive to being smoothed out for test job.It is powered using folding solar charging unit, China's High aititude, the west area that the sunshine-duration is long and intensity is big, not only can be to novel portable liquid cathode glow discharge light It spectrometer and powers in real time for the laptop of data processing, it is energy saving, be conducive to develop to green analytical technology direction; Novel portable spectrometer gross weight is less than 10 kilograms, is also convenient for carrying, and practical value is high, existing convenient for carrying out in western remote districts Field analysis works.
Description of the drawings
Fig. 1 is the schematic device of the utility model;
Wherein:Stent 1, sample solution bottle 2, sample introduction hose 3, waste liquid bottle 4, folding solar charger 5, LiFePO4 Battery pack 6, constant current constant voltage dual pressure controller 7, current-voltage regulator 8, display screen 9, embedded liquid cathode glow discharge knot Structure 10, anode 11, cathode 12, optical filter 13, condenser lens 14, optical fiber 15, high resolution micro CCD spectrometers 16, conduit 17 With laptop 18.
Specific embodiment
The utility model is described in further detail with reference to the accompanying drawings and detailed description:
As shown in Figure 1:A kind of novel portable liquid cathode glow discharge spectrometry, including sampling structure and for Denso It puts, wherein, sampling structure is gravity flow sampling structure, and the gravity flow sampling structure is telescopic and there is hook on top by one Stent 1, sample solution bottle 2, sample introduction hose 3 forms, and the sample solution bottle 2 is hung on the hook on 1 top of stent, sample The bottom connection sample introduction hose 3 of solution bottle 2;The other end of sample introduction hose 3 connects embedded liquid cathode glow discharge structure 10 In cathode 12;The embedded liquid cathode glow discharge structure 10 is connected to current-voltage regulator 8 by conducting wire and shows Show device 9, current-voltage regulator 8 is connected to constant current constant voltage dual pressure controller 7, and constant current constant voltage dual pressure controller 7 is connected by conducting wire Then the anode 11 and cathode 12 in embedded liquid cathode glow discharge structure 10;Connected in the bottom of cathode 12 by conduit 17 Connect waste liquid bottle 4;Aperture is provided on the outer cover of embedded liquid cathode glow discharge structure 10, installs and filters in aperture external application stent Mating plate 13 and focusing transmissive mirror 14 focus on transmissive mirror 14 and pass through the connection CCD detector 16 of optical fiber 15;The CCD detector 16 is logical Data cable is crossed with data handling system to be connected;The preferred laptop 18 of the data handling system;It is described to supply electric installation by folding Formula solar charger 5 connects composition with ferric phosphate lithium cell group 6 by conducting wire;The solar charger 5 is by the collapsible sun It can plate composition.So design can reduce the volume and weight of instrument, easy to carry.
In order to further reduce weight of equipment, in above-described embodiment, it is preferred that the material of the stent 1 is plastics, is drawn For elongation up to 3 meters, load-bearing is at least 1 kilogram.
In order to ensure that waste liquid discharges cathode glow discharging system in time, in above-described embodiment, it is preferred that sample introduction hose 3 is adopted With 1.6 millimeters of outer diameter, the small hose of 1.0 mm pore size of internal diameter, the internal diameter of conduit 17 is at least 2 millimeters.
In order to maintain smoothly to discharge, stable measuring signal is obtained, in above-described embodiment, it is preferred that anode 11 is tungsten Silk, cathode 12 are taper graphite.
In order to improve energy conversion efficiency, reduce equipment volume, in above-described embodiment, it is preferred that folding solar fills For solar panels in electric appliance 5 using imported from America high-efficiency solar plate, solar recharging power peak is 160W.
In order to improve the accuracy of data, while the weight of equipment is reduced, in above-described embodiment, it is preferred that CCD detector 16 be fiber optic conduction high resolution spectrometer CCD, is produced by Ocean Optics companies of the U.S., model HR4000, wavelength is rung Answering scope, resolution ratio is 0.3 nanometer, and weight is 0.57 kilogram for 200~1100 nanometers.
It is so worked using the field in-situ analysis flow of technical solutions of the utility model:
It is live in the wild, each component in Fig. 1 has been linked in sequence, folding solar charger 6 is allowed to give LiFePO4 electricity 6 real time charging of pond group;Prepare the mark of each 1 μ g/mL of Li and K containing the hydrochloric acid or nitric acid medium that volume fraction is 1.0%~1.5% Quasi- solution adjusts condenser lens 14, obtains that Li or K is maximum and most stable of signal strength;Current-voltage regulator 8 is adjusted, really Determine the relation of optimum current and Li, K sensitivity;The sensitivity of test equipment and the relation of acidity, determine optimum acidity;It is sour herein Under degree, compound concentration is 0 (blank), Li, K standard solution of 0.01,0.02,0.05,0.1,0.2,0.5,1 μ g/mL respectively, is counted Calculate calibration curve equation and linearly dependent coefficient;Under this acidity, sample solution is prepared, often tests test one after 5 samples Li, K standard solution of secondary 1 μ g/mL, every 10 sample analysis one divide again.It is molten higher than Li, K sample of 10 μ g/mL for concentration Liquid, signal are present with the situation of saturation, it is necessary to be diluted in 0.01~1 μ g/mL concentration ranges, then accurately measured.

Claims (8)

1. a kind of novel portable liquid cathode glow discharge spectrometry, including sampling structure and for electric installation, it is characterised in that: The sampling structure is gravity flow sampling structure, and the gravity flow sampling structure includes a telescopic and top with extension again Stent (1), sample solution bottle (2) and the sample introduction hose (3) of hook;The sample solution bottle (2) is hung on the extension on stent (1) top On hook, the bottom of the sample solution bottle (2) is fixedly connected with one end of sample introduction hose (3) and the sample introduction hose (3) and sample are molten The inner cavity connection of liquid bottle (2):The other end of the sample introduction hose (3) is connected in embedded liquid cathode glow discharge structure (10) Cathode (12);
The embedded liquid cathode glow discharge structure (10) passes through conducting wire with current-voltage regulator (8) and display (9) Connection, the current-voltage regulator (8) are connected by conducting wire with constant current constant voltage dual pressure controller (7), the constant current constant voltage high pressure Controller (7) is connected by conducting wire with the anode (11) in embedded liquid cathode glow discharge structure (10) and cathode (12); The bottom of the cathode (12) is connected by conduit (17) with waste liquid bottle (4);The embedded liquid cathode glow discharge structure (10) aperture is provided on outer cover, in aperture external application stent installation optical filter (13) and transmissive mirror (14) is focused on, focuses on transmissive mirror (14) it is connected by optical fiber (15) with CCD detector (16);The CCD detector (16) passes through data cable and data handling system It is connected;
It is described to include folding solar charger (5), the folding solar charger (5) and LiFePO4 again for electric installation Battery pack (6) is connected by conducting wire.
2. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described The material of stent (1) is plastics, and for tensile elongation up to 3 meters, load-bearing is at least 1 kilogram.
3. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described Sample introduction hose (3) is using 1.6 millimeters of outer diameter, the small hose of 1.0 mm pore size of internal diameter.
4. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described The internal diameter of conduit (17) is at least 2 millimeters.
5. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described Anode (11) is tungsten filament, and the cathode (12) is taper graphite.
6. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described The charge power peak value of solar panels in folding solar charger (5) is 160W.
7. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1 or 6, it is characterised in that: The solar charger (5) is folding solar plate.
8. a kind of novel portable liquid cathode glow discharge spectrometry according to claim 1, it is characterised in that:It is described CCD detector (16) is fiber optic conduction high resolution spectrometer CCD, and wavelength response range is 200~1100 nanometers, and resolution ratio is 0.3 nanometer, weight is 0.57 kilogram.
CN201721567368.1U 2017-11-22 2017-11-22 A kind of novel portable liquid cathode glow discharge spectrometry Expired - Fee Related CN207379929U (en)

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CN201721567368.1U CN207379929U (en) 2017-11-22 2017-11-22 A kind of novel portable liquid cathode glow discharge spectrometry

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109406493A (en) * 2018-09-21 2019-03-01 中国地质大学(武汉) A kind of portable fluid cathode glow discharging heavy metal detector and detection method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109406493A (en) * 2018-09-21 2019-03-01 中国地质大学(武汉) A kind of portable fluid cathode glow discharging heavy metal detector and detection method

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CF01 Termination of patent right due to non-payment of annual fee

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