CN105572103A - Method for quantitatively detecting multiple heavy metals in leather at same time based on LIBS (Laser-Induced Breakdown Spectroscopy) technology - Google Patents
Method for quantitatively detecting multiple heavy metals in leather at same time based on LIBS (Laser-Induced Breakdown Spectroscopy) technology Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 title claims abstract description 36
- 239000010985 leather Substances 0.000 title claims abstract description 22
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 16
- 238000005516 engineering process Methods 0.000 title abstract description 7
- 230000003595 spectral effect Effects 0.000 claims abstract description 24
- 238000001228 spectrum Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract 2
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- 238000010813 internal standard method Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000004611 spectroscopical analysis Methods 0.000 claims description 2
- 230000005477 standard model Effects 0.000 claims description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 abstract 2
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 26
- 238000000295 emission spectrum Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 101000694017 Homo sapiens Sodium channel protein type 5 subunit alpha Proteins 0.000 description 3
- 238000002679 ablation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005274 electronic transitions Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010606 normalization Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; rubber; leather
- G01N33/447—Leather
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Abstract
The invention discloses a method for quantitatively detecting multiple heavy metals in leather at the same time based on an LIBS (Laser-Induced Breakdown Spectroscopy) technology. The method adopts an LIBS detecting system which is formed by a Q-switched pulse Nd:YAG (Yttrium Aluminum Garnet) laser, an echelle grating spectrometer, an ICCD (Intensified Charge-Coupled Device) detector, a rotating platform and the like. The method comprises the following steps: firstly, regulating laser energy by an energy attenuation system consisting of a half-wave plate and a laser Glan prism, gathering the laser energy on the surface of a sample which is fixed to the rotating platform through a focusing lens, and ablating, gasifying and ionizing substances on the surface of the detected sample, thus forming laser plasma; secondly, obtaining a spectral signal of the laser plasma through a spectrum collection system, analyzing and converting element types corresponding to a spectral line, and obtaining content information of characteristic elements through conversion; thirdly, obtaining concentrations of heavy metal elements by combining a CF (Calibration-free)-LIBS method according to the obtained information of the elements.
Description
Technical field
The present invention relates to the detection technique of heavy metal, particularly a kind of based on LIBS in conjunction with free scaling method simultaneously, the method for quick of various heavy in Quantitative detection leather.
Background technology
Leather products is the staple commodities of Zhejiang Province's outlet, and its output value is all self-evident with outlet status.Heavy metal has huge harm to human body, and there is strict requirement the countries and regions such as European Union, the U.S. to leather heavy metal, detects according to current detection method, and the annual expense produced is huge, also needs to spend the much time simultaneously.And we find in work in the past few years, footwear detects that the ratio of the heavy metals such as Pb, Cd, Cr is not high, and this also just means that we take a large amount of expenses and time in the thing that relative risk is not high.
The detection method of current people's heavy metal element mainly relies on the chemical analysis method and spectroscopic analysis methods that carry out in laboratory, and the method for more common detection contents of heavy metal elements comprises X-ray fluorescence method, atomic absorption spectrography (AAS) and ICP-AES etc.
X-ray fluorescence analysis method can realize quick detection, but its sensitivity is lower, and sample substrate interference is large, atomic absorption spectrography (AAS) and inductively coupled plasma atomic emission spectrum technology have the features such as sensitive, accurate, low-level interference, but equipment is relatively costly, need to clear up process to measurement sample, complicated operation is time-consuming, cannot realize Fast Measurement.
Laser-induced Breakdown Spectroscopy (LaserInducedBreakdownSpectroscopy, LIBS) technology is the new technology that a kind of plasma emission spectrum utilizing high energy pulse Reciprocity of Laser & Materials to produce carries out ultimate analysis.This spectral technique of LIBS and tradition utilize contiguous physical device as atomization driving source atomic emission spectrum technology compared with there is series of advantages, first can realize original position remote measurement.LIBS detection speed can much smaller than 1 second.Another feature of LIBS is exactly that sample does not need pre-service, and sample form is not limit, highly sensitive, can carry out real-time analysis.
But because LIBS is subject to such environmental effects, in quantitative test, also there is larger gap compared with conventional art simultaneously, therefore the research of LIBS heavy metal method for quick in light industrial goods, has extremely important Research Significance and practical value.
Summary of the invention
The object of this invention is to provide a kind of based on LIBS fast, the method for various heavy pollutant in the detection leather of simple, simultaneous quantitative.To solve existing LIBS usually only for inoganic solids sample, and to organic sample be difficult to detect problem.
Existing to contents of heavy metal elements detection technique complex procedures in leather and longer problem consuming time in order to solve, the technical solution adopted in the present invention is:
Detect a method for various heavy in leather based on LIBS simultaneous quantitative, the platform of experimental system comprises: Laser output system, specimen rotating holder, spectral collection system and automated data analysis system.It is characterized in that: the design of rotation platform, in the process of experiment, be placed in by sample on rotation platform, sample can not be punctured by laser pulse, guarantees the collection of plasma spectrum.Next is the optimization to experiment condition.By the Optimization analyses to experiment parameter, we can analyze the content of heavy metal in leather more accurately.Be finally the selection of data divisional processing method, the contrasts such as free scaling method and internal calibration method, conventional strength internal standard method and outer scaling method, the advantage that the method is the most outstanding does not need to adopt a large amount of standard models to obtain typical curve, and process is simple.Overcome the impact of matrix effect on experimental result to a certain extent, degree of accuracy improves.
A kind of method detecting various heavy in leather based on LIBS simultaneous quantitative: the laser beam of above-mentioned Laser output system converges at the surface detecting sample by condenser lens, ablation, gasification, ionization are carried out to the surface mass detecting sample, forms laser plasma.Regulate Laser output system, change the energy of laser beam, make to reach the strongest containing element spectral line in the laser plasma of generation.
A kind of method detecting various heavy in leather based on LIBS simultaneous quantitative: obtain spectrum of laser plasma signal by spectral collection system, now spectrometer is under being operated in external trigger pattern, outside under trigger mode, spectrometer receives the TTL signal of laser instrument as synchronizing signal, and the delay of integral time is synchronous with this input signal.
A kind of method detecting various heavy in leather based on LIBS simultaneous quantitative: measure spectral data signal and be directly imported in computing machine spectrum analysis software package and analyze.
The present invention and traditional leather detection means have following advantages:
1. sample is without the need to pre-service, can realize original position on-line checkingi, is applicable to scene evidence taking task.
2. data analyzing speed is fast, highly sensitive, and precision is high and reproducible.Real-time Detection task can be completed.
3. LIBS can carry out Simultaneous multi element analysis, can not omit any metallic element.Particular/special requirement is not had to sample shape, analysis environments etc.
4. be suitable for the on-site land survey task under complex environment.
Accompanying drawing explanation
Fig. 1 example of the present invention is based on quick, the quantitative detection method square law device schematic diagram of heavy metal in the leather of LIBS.
Fig. 2 specimen rotating holder.
Fig. 3 spectral intensity is with the change curve of time delay.
Fig. 4 spectral intensity changes with depth of focus
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
The present embodiment is the method detecting leather heavy metal based on LIBS.As shown in Figure 1, the LIBS system that experiment adopts forms primarily of parts such as Q impulse Nd:YAG laser instrument, sample stage, digital delay controller, echelle spectrometer, ICCD detecting device and computing machines.Q impulse Nd:YAG laser instrument, the optical maser wavelength 1064nm of the work of employing, pulsewidth is 10ns, repetition frequency 10Hz, single-pulse laser energy 150mJ, the energy attenuation system fading margin that laser energy is made up of 1/2nd wave plates and laser Glan prism, excitation light beam diameter 5mm.
When experiment starts, the 1064nm laser pulse that laser instrument sends reflects through catoptron, then the condenser lens being 175mm through focal length focuses to sample surfaces, spot diameter is about 500 μm, and sample surfaces produces High Temperature High Pressure plasma body of light, and the emission spectrum thereupon produced imports among spectrometer through collecting by fibre-optical probe, spectrometer is middle echelle spectrometer, detection wavelength coverage is 190nm ~ 900nm, and spectrum resolution ability is: λ/Δ λ=15000, and relative aperture is 1/10.Spectrometer coordinates ICCD detector by data storing in computing machine, and the data measured directly are imported in computing machine spectrum analysis software package and analyze.Now spectrometer is under being operated in external trigger pattern, and outside under trigger mode, spectrometer receives the TTL signal of laser instrument as synchronizing signal, and the delay of integral time is synchronous with this input signal.Control whole LIBS by PC to test.Experiment is carried out under normal temperature and pressure conditions, is protection and the normal use of exact instrument, relative air humidity < 40%.
Need in experiment to be optimized the parameter of experiment.The formation of laser induced plasma needs pulsed laser energy to exceed certain threshold value.When pulsed laser energy exceedes threshold value, line strength starts linearly to improve with laser energy, finally occurs saturated phenomenon.In experiment, the intensity of analytical element spectral line and the relation of pulsed laser energy find, line strength with pulsed laser energy monotone increasing, single laser pulse in maximal value time there is not saturated phenomenon yet.Therefore in order to obtain spectral line strong as far as possible, energy of lasers is set to maximal value.
The laser induced plasma initial stage spectral line of emission there is strong continuous background interference and noise ratio is larger, spectral line noise when signal-to-background ratio can be improved by delay measurements. Fig. 3 be arrange ICCD gather gate-width be 1 μ s time, in sample, element spectral line of emission intensity gathers the changing trend diagram of time delay. as seen from the figure, along with the increase of time delay during beginning, line strength increases fast; When delay time is at 1 μ s, line strength reaches the strongest. and decline gradually more than the intensity both during 1 μ s, in order to collect the strongest line strength, comprehensively both consideration, the time delay adopted in experiment is 1 μ s.
The focus of lens is called depth of focus to the distance of sample, also be the principal element affecting the spectral line of emission. be provided with a series of depth of focus value in an experiment respectively :-3mm ,-2mm ,-1mm, 0mm, 1mm, 2mm, 3mm, record spectral line of emission intensity, obtained by Fig. 4, at identical conditions, during depth of focus 2mm, the intensity of the spectral line of emission is the strongest, therefore selects 2mm as best depth of focus condition.
Can remove the impurity on measured matter surface by the ablation effect of laser or excite the impact of impurity in air in LIBS, so take the number of times that laser pulse repeatedly adds up in an experiment, experiment condition be the cumulative effects of 20 times.Record several LIBS spectrograms of often kind of sample, every width spectrogram is the average result that 20 laser pulses act on sample surfaces difference.Each laser pulse impact sample surfaces zones of different, improves spectral quality.
Obtain the laser-induced breakdown plasma spectrum figure of sample by experiment, the wavelength of various element in sample and corresponding light intensity can be obtained in spectrogram.When plasma is in local thermal equilibrium, the electron density of excited state is relevant with the total concentration of the ion of this element, and the electron density of excited state is proportional to again corresponding line strength.So the intensity of the spectral line of emission can be expressed as:
In formula: λ is the characteristic spectral line wavelength of selection analysis; The low-lying level that the high level that k is the electronic transition that characteristic wavelength is corresponding, i are the electronic transition that characteristic wavelength is corresponding, I is the line strength measured; A
kifor k energy level is to the transition probability of i energy level, E
kfor high level energy, g
kfor high level degeneracy, k
bfor Boltzmann constant, C
sfor the atom content corresponding to this emission line, U
s(T
e) be partition function, T
efor plasma electron temperature, F is test parameters.
Here we first can be defined as follows parameter:
Can be reduced to: y=mx+q
s
To often kind of element in sample, linear fit (being called Boltzmann oblique line) is carried out to the data point of many spectral lines detected, obtains plasma electron temperature T by the slope of Boltzmann oblique line
e, can obtain
Intercept q corresponding to each element also can be obtained by Boltzmann oblique line
s, F tries to achieve by the normalization of all elements concentration in sample:
Concentration computing formula is:
The experiment parameter that the partition function corresponding according to different element and normalization are tried to achieve, can try to achieve the concentration of heavy metal element in sample.
Above content is the further description done the present invention in conjunction with optimal technical scheme, can not assert that the concrete enforcement of invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, do not departing under concept thereof of the present invention, making simple deduction and replacement, all should be considered as protection scope of the present invention.
Claims (5)
1. detect a method for various heavy in leather based on LIBS simultaneous quantitative, the platform of experimental system comprises: Laser output system, specimen rotating holder, spectral collection system and automated data analysis system.It is characterized in that: the first design of rotation platform, in the process of experiment, be placed in by sample on rotation platform, organic sample can not be punctured by laser pulse, guarantees the collection of plasma spectrum.Next is the optimization to experiment condition.By the Optimization analyses to experiment parameter, we can analyze the content of heavy metal in leather more accurately.Be finally the selection of data analysis processing method, the contrasts such as free scaling method and internal calibration method, conventional strength internal standard method and outer scaling method, the advantage that the method is the most outstanding does not need to adopt a large amount of standard models to obtain typical curve, and process is simple.Overcome the impact of matrix effect on experimental result to a certain extent, degree of accuracy has had raising.
2. a kind of method detecting various heavy in leather based on LIBS simultaneous quantitative according to claim 1, it is characterized in that: what adopt in Laser output system is Q impulse Nd:YAG laser instrument, the optical maser wavelength 1064nm of the work adopted, pulsewidth is 10ns, repetition frequency 10Hz, single-pulse laser energy 150mJ, the energy attenuation system fading margin that laser energy is made up of 1/2nd wave plates and laser Glan prism, excitation light beam diameter 5mm.In order to reduce the impact of self absorption effect and reduce the non-equal Uniform of sample surfaces to the impact of experimental result, Laser Focusing is made to be about 500 μm at the spot diameter of sample surfaces.
3. a kind of method detecting various heavy in leather based on LIBS simultaneous quantitative according to claim 1, it is characterized in that: existing LIBS usually only for the experiment of inoganic solids sample, and detects seldom organic sample.Organic sample can often there will be the phenomenon punctured in an experiment, derivative spectomstry collection system can not the spectrum of collection element.By the adjustment to rotation platform rotational speed and laser energy, above-mentioned problem can be efficiently solved.
4. a kind of method detecting various heavy in leather based on LIBS simultaneous quantitative according to claim 1, it is characterized in that: before obtaining spectral information, the parameter of experiment is optimized, such as laser energy 60mJ, time delay 1 μ s, depth of focus 2mm, laser spot diameter to be about the number of times 20 that 500 μm and laser pulse repeatedly add up inferior.Further increase the precision of experiment.For protection and the normal use of exact instrument, relative air humidity < 40%.
5. a kind of method detecting various heavy in leather based on LIBS simultaneous quantitative according to claim 1, it is characterized in that: the Laser-induced Breakdown Spectroscopy data that the spectroscopic data of collection imports each element in computing machine and database into are compared, analyze the element kind conversed corresponding to spectral line, and pass through the content information of the characteristic element that conversion obtains.According to the information of the element obtained, calculate the concentration that simultaneously can obtain detection device for multi metallic elements in conjunction with free scaling method.
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| CN106442433A (en) * | 2016-09-29 | 2017-02-22 | 哈尔滨理工大学 | Polymer breakdown luminescent spectrum measurement system based on ICCD imaging |
| CN106596514A (en) * | 2017-01-24 | 2017-04-26 | 浙江大学 | Blade-heavy-metal-content detection method with moisture content corrected based on Ca element ratio |
| CN106769882A (en) * | 2016-11-01 | 2017-05-31 | 深圳先进技术研究院 | Spilled oil monitoring instrument and its monitoring method |
| CN108303410A (en) * | 2018-04-23 | 2018-07-20 | 南京信息工程大学 | Trace element and its isotope automatic checkout system |
| CN109596601A (en) * | 2018-12-24 | 2019-04-09 | 河钢股份有限公司 | A kind of device and method of rapid Optimum laser induced breakdown spectroscopy lens distance |
| CN110487774A (en) * | 2019-10-09 | 2019-11-22 | 南京信息工程大学 | Laser induced breakdown spectroscopy (LIBS) water quality quality evaluation system |
| CN110672586A (en) * | 2019-10-28 | 2020-01-10 | 岭澳核电有限公司 | Concrete corrosion state detection method based on LIBS |
| CN111398253A (en) * | 2020-03-17 | 2020-07-10 | 浙江大学 | Atmosphere-adjustable L IBS signal enhancement device and heavy metal detection method |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442433A (en) * | 2016-09-29 | 2017-02-22 | 哈尔滨理工大学 | Polymer breakdown luminescent spectrum measurement system based on ICCD imaging |
| CN106769882A (en) * | 2016-11-01 | 2017-05-31 | 深圳先进技术研究院 | Spilled oil monitoring instrument and its monitoring method |
| CN106596514A (en) * | 2017-01-24 | 2017-04-26 | 浙江大学 | Blade-heavy-metal-content detection method with moisture content corrected based on Ca element ratio |
| CN106596514B (en) * | 2017-01-24 | 2019-07-16 | 浙江大学 | Blade heavy metal content detection method based on Ca element ratios correction moisture content |
| 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 |
| CN109596601A (en) * | 2018-12-24 | 2019-04-09 | 河钢股份有限公司 | A kind of device and method of rapid Optimum laser induced breakdown spectroscopy lens distance |
| CN109596601B (en) * | 2018-12-24 | 2024-03-22 | 河钢股份有限公司 | Device and method for rapidly optimizing laser-induced breakdown spectroscopy lens distance |
| CN110487774A (en) * | 2019-10-09 | 2019-11-22 | 南京信息工程大学 | Laser induced breakdown spectroscopy (LIBS) water quality quality evaluation system |
| CN110672586A (en) * | 2019-10-28 | 2020-01-10 | 岭澳核电有限公司 | Concrete corrosion state detection method based on LIBS |
| CN111398253A (en) * | 2020-03-17 | 2020-07-10 | 浙江大学 | Atmosphere-adjustable L IBS signal enhancement device and heavy metal detection method |
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Application publication date: 20160511 |