CN208283281U - Trace element and its isotope automatic checkout system - Google Patents
Trace element and its isotope automatic checkout system Download PDFInfo
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- CN208283281U CN208283281U CN201820586031.3U CN201820586031U CN208283281U CN 208283281 U CN208283281 U CN 208283281U CN 201820586031 U CN201820586031 U CN 201820586031U CN 208283281 U CN208283281 U CN 208283281U
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- induced breakdown
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Abstract
The utility model discloses a trace elements and its isotope automatic checkout systems, including sample pretreatment apparatus, laser-induced breakdown spectroscopy device, infrared spectrometer and PC machine, the sample pretreatment apparatus, laser-induced breakdown spectroscopy device are sequentially arranged on sample conveyer belt between infrared spectrometer, the laser-induced breakdown spectroscopy device and infrared spectrometer are provided with oxidation unit between the laser-induced breakdown spectroscopy device and infrared spectrometer with PC machine data connection.The utility model is by combining infrared spectrum technology with laser induced breakdown spectroscopy, the mass spectrometric data of test substance and the atomic emissions spectrum of element can be obtained, after being analyzed by data, the valid data of the essential information of the type and content of heavy metal element and heavy metal element isotope in the substance can be obtained, to in substance, trace element composition confirms, greatly improves the accuracy and sensitivity of substance detection.
Description
Technical field
The utility model relates to trace element detection devices, and in particular to a trace elements and its isotope detect automatically
System.
Background technique
There is many kinds of substance in nature, element is the important component of substance.In people's daily life, meeting
Various elements is touched, such as carbon, hydrogen, oxygen these infrastructure elements, also just like heavy metal elements such as iron, copper, zinc.In group
At in the element of substance, type numerous and complicated, have it is beneficial to human body, even if also there is quite a few element content to be seldom
Have to health and greatly threaten the heavy metal such as lead, mercury, therefore establishes the elemental analysis detection system of complete set,
Production and living to people are a highly important things.
Current element analysis technology, such as laser induced breakdown spectroscopy (LIBS), Fourier transform infrared spectroscopy
Technology, laser-induced fluorescence spectroscopy technology etc. are capable of the element composition of detecting material, such as near infrared spectrum Detection Techniques,
Due to the mass number difference of molecule, can be determined by the ultra-red vibration frequency of different functional groups in measurement substance substance at
Point, if the vibration frequency of-O-H of ordinary liquid water is 1603.036cm-1, 3816.884cm-1, 3922.046cm-1, and heavy water
In-D-H vibration frequency be 1172.400cm-1, 2753.440cm-1, 2876.700cm-1;The oxide of mass number 220204PbO vibration frequency is 711.650cm-1, the oxide of mass number 222206PbO vibration frequency is 711.400cm-1;Mass number
223 oxide207PbO vibration frequency is 715.930cm-1, and the oxide that mass number is 224208PbO vibration frequency is
711.270cm-1Generally it is lower than207PbO.The red oxide external spectrum vibration frequency of several isotope species is completely different therefore red
External spectrum technology can detect to obtain the Isotope Information of substance.But it is limited in that the mass number information for only passing through substance,
Single atom cannot be analyzed by being directed to micel, can not obtain the atomic emission spectrum information of material element, analysis
Precision is not high enough, and the effective information of acquisition is limited, cannot achieve high accurately element on-line analysis.Meanwhile even if current spy
Survey technology can be realized multicomponent element detection, but the sensitivity of its detection is not high, especially when object element content is lower
When, accurately detection result can not be provided.
Utility model content
Purpose of utility model: the purpose of the utility model is to provide a trace elements and its automatic detection systems of isotope
System, the existing detection and analysis precision of solution is not high, and acquisition element information is limited, the accuracy of substance detection and asking for poor sensitivity
Topic.
Technical solution: trace element and its isotope automatic checkout system described in the utility model, including specimen preprocessing
Manage device, laser-induced breakdown spectroscopy device, infrared spectrometer and PC machine, the sample pretreatment apparatus, laser-induced breakdown
It is sequentially arranged between spectral device, infrared spectrometer on sample conveyer belt, the laser-induced breakdown spectroscopy device and infrared
Spectrometer with PC machine data connection, is provided with oxidation dress between the laser-induced breakdown spectroscopy device and infrared spectrometer
It sets.
In order to improve detection accuracy, the sample pretreatment apparatus includes grinder, dryer and cooked flake wrapping machine and successively sets
It sets on sample conveyer belt.
The solid sample after grinding is delivered to next device for convenience, the grinder outlet is provided with sample and holds
Device.
In order to improve scanning speed and guarantee the whole letters for all frequencies that can obtain radiation source in any time of measuring
Breath, the infrared spectrometer are Fourier Transform Infrared Spectrometer.
In order to facilitate the oxidation of trace element isotope, the oxidation unit includes oxidizing chamber, is provided in the oxidizing chamber
Heat fulgurite, oxygen jet and air extractor.
The utility model has the advantages that the utility model is by combining infrared spectrum technology with laser induced breakdown spectroscopy, energy
The mass spectrometric data of test substance and the atomic emissions spectrum of element are enough obtained, after being analyzed by data, can be obtained in the substance
The essential information of the type and content of heavy metal element and the valid data of heavy metal element isotope, to trace member in substance
Element composition is confirmed, the accuracy and sensitivity of substance detection are greatly improved.The utility model can be detected automatically solid
Various substances under body fluid body different conditions, no longer need in whole process to carry out sample processing and during detection
Preferable signal-to-noise ratio can be obtained, the substance classes of detection are effectively expanded, improves the comprehensive of detection.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of Tthe utility model system;
Fig. 2 is the flow diagram of the utility model detection method;
Fig. 3 is the structural schematic diagram of oxidation unit.
Specific embodiment
The utility model is described in further detail with reference to the accompanying drawing.
As shown in Figure 1-3, trace element and its isotope automatic checkout system, including sample pretreatment apparatus, laser lure
Lead breakdown spectral device 1, infrared spectrometer 2 and PC machine 5, it is sample pretreatment apparatus, laser-induced breakdown spectroscopy device 1, infrared
It is sequentially arranged between spectrometer 2 on sample conveyer belt 3, laser-induced breakdown spectroscopy device 1 and infrared spectrometer 2 are and PC machine
5 data connections are provided with oxidation unit 4 between laser-induced breakdown spectroscopy device 1 and Fourier Transform Infrared Spectrometer 2.Sample
Product pretreatment unit includes grinder 9, dryer 8 and cooked flake wrapping machine 7 and is successively set on sample conveyer belt 3, the sample of solid
Successively solid sample is ground by grinder, convenient for reacting sample sufficiently in oxidation process later, if sample surfaces
Very coarse, when carrying out laser ablation, signal is not that very obviously, the accuracy of detection will decline.Dryer be in order to
By the extra moisture removal in sample, because the moisture in sample has stronger self-priming to laser when carrying out laser ablation
It produces effects and answers, the signal-to-noise ratio of signal can be seriously affected.The effect of cooked flake wrapping machine is in order to by smashed sample curable type, because in high energy
Under the ablation effect for measuring laser, the sample of crushing is easy to be broken up, and then influences signal.Grinder outlet is provided with sample and holds
Device, solid sample are placed directly in grinder, and after grinding, the vessel for holding solid sample, example are had in outlet
Such as culture dish or other small-sized apparatus for placing), it is transmitted later with conveyer belt, so setting facilitates sample to transmit with sample
Artificial workload is reduced with 3 movements.Oxidation unit 4 includes oxidizing chamber, is provided with heating fulgurite in oxidizing chamber, oxygen jet and
Air extractor.Fulgurite external cord is heated, oxygen jet connects oxygen air pump, and air extractor connects mechanical pump.When sample is completed
After previous step Laser ablation procedures, under the running of conveyer belt, sample is transported in the oxidizing chamber of oxidation unit, is transmitted later
Band 3 is stagnated, former and later two closing doors 12 of oxidizing chamber are turned off manually at this time, will aoxidize indoor sky by air extractor 11 later
Gas discharge, to which after a certain period of time, heating fulgurite 10 of the starting in oxidizing chamber carries out heating heating to entire oxidizing chamber, add
While hot, oxygen valve is opened, so that certain density oxygen is transported in oxidizing chamber by oxygen jet 13, with sample to be tested
Carry out oxidation reaction.After reacting the regular hour, heating tube power supply is closed, closes oxygen air pump, opens oxidizing chamber closing door,
Conveyer belt starts operation at this time, and the sample to be tested after being oxidized is delivered to next device, carries out next operation.
Wherein, laser-induced breakdown spectroscopy device is issued the laser of central wavelength 1064nm by Nd:YAG laser first,
The Nd:YAG that another beam center wavelength is 1064nm reheats light source as plasma.Four-way digital delay impulse generator
The time interval of two beam Laser emissions is controlled in 1 μ s, the first beam laser pulse is by focal length f1 after total reflection mirror M reflection
The plano-convex lens of 50mm act on sample to be tested, are through another focal length f2 after another beam laser pulse is separated by certain time later
The plano-convex lens of 50mm are acted on plasma after assembling and are reheated.Plasma resonance signal is after fiber optic collector is collected
Coupled into optical fibres, signal are divided by grating spectrograph, are finally detected by computer software to signal, and element is obtained
Atomic emission spectrum, the element of sample to be tested composition and content are detected.Fourier Transform Infrared Spectrometer device base
This structure has three parts: front-end system, interferometer system, data acquisition and processing system.Incident light is divided by infrared light supply
Two equal beam coherent lights of intensity: it is a branch of to be transmitted to movable plane reflecting mirror M1 through beam splitter B, and returned to after being reflected by M1
Beam splitter B;Another beam arrives plane mirror M2 after beam splitter reflects, after be reflected back toward beam splitter B, M2 ' is parallel with M1, then two
Shu Guang meets interfere again.When M1 is mobile, two-beam optical path difference changes, later by focus lamp L3 interferometer
After the light beam of injection is assembled, detector C is injected, interference light intensity signal is converted electric signal by detector.Pass through the device energy
The Isotope Information and its design feature of enough preliminary acquisition samples to be tested.
When being detected using the utility model, sample to be tested is handled by sample pretreatment apparatus, if sample is
Solid then passes through grinding device, drying unit and cake of press device, and final cake of press sizing directly passes through baking if sample is liquid
Dry, the final cake of press molding of cake of press device;The molding sample to be tested of cake of press is delivered to laser induced breakdown spectroscopy by sample delivery band
Device carries out laser ablation under the 1064nm laser beam focus effect that pulsed YAG laser generates, and material surface can moment
The plasma flame of high temperature is generated, and rapid cooling is transitted to low-lying level state by the substance of plasmoid, thus meeting
Energy is given off outward, these information correspond to different spies according to different types of element by being collected by fiber spectrometer
Peak is levied, the atomic emission spectrum of material element is obtained after being handled by PC machine, is able to carry out quick analysis, obtains the object of sample to be tested
The preliminary data of prime element type and content;Sample is delivered to oxidation unit by conveyer belt later, and sample conveys after being oxidized
To infrared spectrometer, trace element is oxidized in oxidation unit, is conducive to Fourier transform infrared spectroscopy and is detected, Fu Li
There are the vibration frequencies of different infrared spectroscopies according to the substance of different quality number for leaf transformation infrared spectrometer, to obtain sample
The isotope mass spectrometry data of substance are simultaneously sent to PC machine, can be believed by these information with the main component of quick obtaining test substance
Breath and chemical species that may be present complete composition measurement and composition prediction;Last PC machine is according to the atomic emissions of trace element
Spectrum and the MASS SPECTRAL DATA ANALYSIS of its isotope obtain the type and content and isotope structure letter of the trace element in sample to be tested
Breath.
The utility model can obtain the spectra count of test substance by combining infrared spectrum technology with LIBS technology
Accordingly and the atomic emissions of element are composed, and after analyzing by data, can obtain the type and content of heavy metal element in the substance
Essential information and heavy metal element isotope valid data, in substance heavy metal element composition carry out further it is true
Recognize, greatly improves the accuracy and sensitivity of substance detection.With LIBS technology, the original of heavy metal element in substance can be obtained
Sub- emission spectra, for finally determining that material composition has more accurate preliminary analysis.Compared with traditional single-pulse laser, adopt
Laser ablation, spectral intensity obtained are carried out to sample to be tested with orthogonal double-pulse laser induced breakdown spectral technology is reheated
It can be effectively improved.Double-pulse laser is able to extend the die-away time of characteristic spectral line spectral intensity, effectively improves letter
Back ratio.In addition, orthogonal dipulse can be improved the detection sensitivity of LIBS technology, the detection limit of element is reduced, member is greatly enhanced
The precision of element detection.Hundreds times faster than traditional infrared spectral instrument of the scanning speed of Fourier Transform Infrared Spectrometer, and
The all information of all frequencies of radiation source can be obtained in any time of measuring, i.e., it is so-called " multiplexing ".For steady
Fixed sample generally obtains interference pattern using Multiple-Scan, cumulative averaging method in one-shot measurement, and the signal-to-noise ratio of signal obtains
Improve.In addition, Fourier Transform Infrared Spectrometer is in entire spectral region up to 0.1cm-1~0.005cm-1.Its point
Resolution is related with the optical path difference of instrument, and optical path difference is bigger, and the resolution ratio of instrument is higher.Therefore Fourier transform infrared spectroscopy detection
Technology detectivity with higher can obtain the mass spectrometric data and structural information of isotope.
Claims (5)
1. a trace elements and its isotope automatic checkout system, which is characterized in that lured including sample pretreatment apparatus, laser
Lead breakdown spectral device (1), infrared spectrometer (2) and PC machine (5), the sample pretreatment apparatus, laser induced breakdown spectroscopy
It is sequentially arranged between device (1), infrared spectrometer (2) on sample conveyer belt (3), the laser-induced breakdown spectroscopy device
(1) and infrared spectrometer (2) with PC machine (5) data connection, the laser-induced breakdown spectroscopy device (1) and infrared spectrometer
(2) oxidation unit (4) are provided between.
2. trace element according to claim 1 and its isotope automatic checkout system, which is characterized in that the sample is pre-
Processing unit includes grinder (9), dryer (8) and cooked flake wrapping machine (7) and is successively set on sample conveyer belt (3).
3. trace element according to claim 2 and its isotope automatic checkout system, which is characterized in that the grinder
(9) outlet is provided with sample holding device.
4. trace element according to claim 1 and its isotope automatic checkout system, which is characterized in that the infrared light
Spectrometer (2) is Fourier Transform Infrared Spectrometer.
5. trace element according to claim 1 and its isotope automatic checkout system, which is characterized in that the oxidation dress
It sets including oxidizing chamber, heating fulgurite (10), oxygen jet (13) and air extractor (11) is provided in the oxidizing chamber.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108303410A (en) * | 2018-04-23 | 2018-07-20 | 南京信息工程大学 | Trace element and its isotope automatic checkout system |
CN114295604A (en) * | 2021-12-30 | 2022-04-08 | 华中科技大学 | Rapid soil nutrient detection system and method for LIBS and NIRS spectrum synchronous acquisition |
-
2018
- 2018-04-23 CN CN201820586031.3U patent/CN208283281U/en active Active
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108303410A (en) * | 2018-04-23 | 2018-07-20 | 南京信息工程大学 | Trace element and its isotope automatic checkout system |
CN108303410B (en) * | 2018-04-23 | 2023-06-23 | 南京信息工程大学 | Trace element and isotope automatic detection system thereof |
CN114295604A (en) * | 2021-12-30 | 2022-04-08 | 华中科技大学 | Rapid soil nutrient detection system and method for LIBS and NIRS spectrum synchronous acquisition |
CN114295604B (en) * | 2021-12-30 | 2024-02-02 | 华中科技大学 | LIBS and NIRS spectrum synchronous acquisition soil nutrient rapid detection system and method |
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