CN102116739A - Nondestructive testing method for absorption coefficient and refractive index of pesticide - Google Patents
Nondestructive testing method for absorption coefficient and refractive index of pesticide Download PDFInfo
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- CN102116739A CN102116739A CN 201010591360 CN201010591360A CN102116739A CN 102116739 A CN102116739 A CN 102116739A CN 201010591360 CN201010591360 CN 201010591360 CN 201010591360 A CN201010591360 A CN 201010591360A CN 102116739 A CN102116739 A CN 102116739A
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Abstract
The invention discloses a nondestructive testing method for absorption coefficient and refractive index of a pesticide. The method comprises the following steps of: testing nitrogen and a pesticide test sample by using a transmission-type terahertz time domain spectroscopy (THz-TDS) to obtain time domain spectrums of the nitrogen and the pesticide test sample respectively; and performing data processing to obtain refractive index spectrum and absorption spectrum of the pesticide test sample at the THz wave band of between 0 and 2.5THz, wherein the pesticide comprises chlorpyriphos methyl, baygon and fenvalerate. By the method, rapid nondestructive testing of the pesticide can be realized; and the method has the advantages of simple sample preprocessing, easiness of operation, high repeatability, simple data processing, relatively accurate testing result and the like. The method has great significance to detection of pesticide residue on fruits and vegetables by using the terahertz time domain technology based on fingerprint spectrums of the three pesticides obtained by the method.
Description
Technical field
The present invention relates to utilize the method for terahertz time-domain spectroscopic technology Pesticides Testing, relate in particular to a kind of absorption coefficient of pesticide and the lossless detection method of refractive index.
Background technology
Chlorpyrifos-methyl, English trade name Chlorpyriphos methyl, it is a kind of organophosphorus insecticide of wide spectrum.Molecular formula C
7H
7Cl
3NO
3PS, molecular weight 322.53,45.5 ℃ of fusing points, former medicine are white crystalline powder.Be used for preventing and treating the insect of storage cereal and the insect of various leaf class crops, also can prevent and treat mosquito adult, fly class, aquatic larva etc.Arprocarb, English trade name Baygon, molecular formula C
11H
15NO
3, molecular weight 209.13, former medicine are white crystalline powder, are dissolved in most organic solvent.Can kill vermin, insect and storage pests such as mosquito, fly, cockroach.Fenvalerate, English trade name Fenvalerate, molecular formula C
25H
22ClNO
3, molecular weight 419.91, former medicine are white crystalline powder, and be water-soluble hardly, is dissolved in dimethylbenzene, acetone and other organic solvent.Be used to prevent and treat cotton, fruit tree, vegetables and other crops insect.
These three kinds of pesticides all belong to poisonous and harmful substance, should note protection during use, avoid sucking or contacting with skin.Along with modern agriculture is growing to the dependence of pesticide, people also more and more pay close attention to the pesticide residues in the food.People all find the residual and metabolin of vestige of pesticide in soil and fruit at present.Because the security that people worry food on the market, the detection of the residual quantity of herbicide has caused the public's extensive concern in the food.All there is the requirement of the high residue weight range of pair pesticide countries in the world, and China does not also have to detect in the fruits and vegetables standard method of pesticide at present.
Existing insecticide residues detection method is broadly divided into vapor-phase chromatography, GC-MS(gas chromatography-mass spectrography) etc.The sample pre-treatments of these class methods is complicated and consuming time, is difficult to the visual inspection of realization to pesticide.Therefore be necessary to set up a kind of detection method quick, accurate, directly perceived, highly sensitive in the fruits and vegetables that detects.In recent years, along with the fast development of THz technology, and its special performance, it can be applied to the Pesticides Testing area research.2009, face will just waited the people to utilize the terahertz time-domain spectroscopy system testing to obtain the tera-hertz spectra of fungicide tebuconazole and own azoles alcohol.2010, people such as Hua Yuefang studied the absorbance of cyfloxylate in the normal hexane solvent, and the correlation technique of quantum chemistry is applied to tera-hertz spectra.2007, three research institutions of Japan announced the tera-hertz spectra of about 500 kinds of materials, comprising the common agricultural chemicals of a part.Terahertz time-domain spectroscopic technology is applied to the Pesticides Testing field at present progressively to be carried out.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of absorption coefficient of pesticide and the lossless detection method of refractive index are provided.
The step of the absorption coefficient of pesticide and the lossless detection method of refractive index is as follows:
1) be that 98～100% pesticide sample and tygon place vacuum drying chamber to dry respectively 2～3 hours with mass percent, getting mass percent and be 50～100% pesticide sample and tygon mixes the back and grinds, depress to the disc thin slice that diameter is 13 mm with sheeter at the pressure of 20～30 MPa, obtain the pesticide specimen;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the time domain waveform of THz wave, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the pesticide specimen is tested, obtain the time domain waveform of its THz wave, as pesticide specimen signal, triplicate is averaged;
4) mean value of reference signal and the mean value of pesticide specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of pesticide specimen signal;
5) employing is extracted the absorption coefficient of pesticide specimen based on the data processing model of fresnel formula
And refractive index
,
In formula (1) and (2), be respectively the ratio and the phase differential of the amplitude of pesticide specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of pesticide specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency;
The light path of test environment: THz is filled with nitrogen, and relative humidity is less than 4.0% in the case.
Described pesticide sample is: chlorpyrifos-methyl, arprocarb and fenvalerate.
The frequency of described chlorpyrifos-methyl
Be 0.4-1.6 THz, the frequency of arprocarb
Be 0.4-1.8 THz, the frequency of fenvalerate
Be 0.4-2.0 THz.
The present invention can realize to agricultural chemicals fast, Non-Destructive Testing, and it is simple to have sample pre-treatments, easy to operate, good reproducibility, advantage such as data processing is simple, and test result is relatively accurate.On the basis of three kinds of pesticide dactylograms that utilize the present invention to obtain, to utilizing the pesticide on the terahertz time-domain technology for detection fruit and vegetable using residual significant.
Description of drawings
Fig. 1 is the terahertz time-domain figure of chlorpyrifos-methyl;
Fig. 2 is the absorption spectra and the spectrum of refractive index of chlorpyrifos-methyl;
Fig. 3 is the terahertz time-domain figure of arprocarb;
Fig. 4 is the absorption spectra and the spectrum of refractive index of arprocarb;
Fig. 5 is the terahertz time-domain figure of fenvalerate;
Fig. 6 is the absorption spectra and the spectrum of refractive index of fenvalerate.
Embodiment
The femto-second laser that terahertz time-domain spectroscopy of the present invention (THz-TDS) STS system test set is made by U.S. Coherent company and the Model Z-1 type THz system of U.S. Zomega company development are formed.It is 800 nm that titanium sapphire femtosecond mode locking pulse laser instrument produces centre wavelength, and the LASER Light Source of pulse width 100 fs, repetition frequency are 80 MHz, and output power is 960 mW.
Test at room temperature (about 294 K) is carried out, and the light path of THz is filled with nitrogen, and relative humidity is about 4.0% in the case.In the scanning process of signal, signal to noise ratio (S/N ratio) is better than 1000 dB, and spectral resolution is better than 10GHz.
The step of the absorption coefficient of pesticide and the lossless detection method of refractive index is as follows:
1) be that 98～100% pesticide sample and tygon place vacuum drying chamber to dry respectively 2～3 hours with mass percent, getting mass percent and be 50～100% pesticide sample and tygon mixes the back and grinds, depress to the disc thin slice that diameter is 13 mm with sheeter at the pressure of 20～30 MPa, obtain the pesticide specimen;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the time domain waveform of THz wave, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the pesticide specimen is tested, obtain the time domain waveform of its THz wave, as pesticide specimen signal, triplicate is averaged;
4) mean value of reference signal and the mean value of pesticide specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of pesticide specimen signal;
5) employing is extracted the absorption coefficient of pesticide specimen based on the data processing model of fresnel formula
And refractive index
,
In formula (1) and (2)
, be respectively the ratio and the phase differential of the amplitude of pesticide specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of pesticide specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency;
The light path of test environment: THz is filled with nitrogen, and relative humidity is less than 4.0% in the case.
Described pesticide sample is: chlorpyrifos-methyl, arprocarb and fenvalerate.
The frequency of described chlorpyrifos-methyl
Be 0.4-1.6 THz, the frequency of arprocarb
Be 0.4-1.8 THz, the frequency of fenvalerate
Be 0.4-2.0 THz.
Embodiment 1
1) chlorpyrifos-methyl sample and the tygon with AG places vacuum drying chamber to dry respectively 2 hours, getting mass percent and be 50% chlorpyrifos-methyl sample and tygon mixes the back and grinds, depress to the disc thin slice that diameter is 13 mm with sheeter at the pressure of 30 MPa, obtain the specimen of chlorpyrifos-methyl;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the THz wave time domain waveform of nitrogen, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the chlorpyrifos-methyl specimen is tested, obtain the time domain waveform of its THz wave, as the sample signal of chlorpyrifos-methyl, triplicate is averaged;
4) mean value of reference signal and the mean value of chlorpyrifos-methyl specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of chlorpyrifos-methyl specimen signal;
5) employing is extracted the absorption coefficient and the refractive index of chlorpyrifos-methyl specimen based on the data processing model of fresnel formula,
In formula (1) and (2), be respectively the ratio and the phase differential of the amplitude of chlorpyrifos-methyl specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of chlorpyrifos-methyl specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency; The frequency of chlorpyrifos-methyl
Be 0.4-1.6 THz.
1) be that 98% arprocarb sample and tygon place vacuum drying chamber to dry respectively 2 hours with mass percent, getting mass percent and be 50% pesticide sample and tygon mixes the back and grinds, depress to the disc thin slice that diameter is 13 mm with sheeter at the pressure of 30 MPa, obtain the specimen of arprocarb;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the THz wave time domain waveform of nitrogen, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the arprocarb specimen is tested, obtain the time domain waveform of its THz wave, as the sample signal of arprocarb, triplicate is averaged;
4) mean value of reference signal and the mean value of arprocarb specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of arprocarb specimen signal;
5) employing is extracted the absorption coefficient and the refractive index of arprocarb agricultural chemicals specimen based on the data processing model of fresnel formula,
（2）
In formula (1) and (2), be respectively the ratio and the phase differential of the amplitude of arprocarb specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of arprocarb specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency; The frequency of arprocarb
Be 0.4-1.8 THz.
The light path of test environment: THz is filled with nitrogen, and relative humidity is less than 4.0% in the case.
Embodiment 3
1) is that 98% fenvalerate sample places vacuum drying chamber to dry 3 hours with mass percent, the fenvalerate sample is ground, depress to the disc thin slice that diameter is 12 mm at the pressure of 20 MPa, obtain the specimen of fenvalerate with sheeter;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the time domain waveform of the THz wave of nitrogen, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the specimen of fenvalerate is tested, obtain the time domain waveform of its THz wave, as fenvalerate specimen signal, triplicate is averaged;
4) mean value of reference signal and the mean value of fenvalerate specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of fenvalerate specimen signal;
5) employing is extracted the absorption coefficient and the refractive index of fenvalerate specimen based on the data processing model of fresnel formula,
In formula (1) and (2)
, be respectively the ratio and the phase differential of the amplitude of fenvalerate specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of fenvalerate specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency; The frequency of fenvalerate
Be 0.4-2.0 THz.
The light path of test environment: THz is filled with nitrogen, and relative humidity is less than 4.0% in the case.
Claims (3)
1. the lossless detection method of the absorption coefficient of a pesticide and refractive index is characterized in that its step is as follows:
1) be that 98～100% pesticide sample and tygon place vacuum drying chamber to dry respectively 2～3 hours with mass percent, getting mass percent and be 50～100% pesticide sample and tygon mixes the back and grinds, depress to the disc thin slice that diameter is 13 mm with sheeter at the pressure of 20～30 MPa, obtain the pesticide specimen;
2) utilize the terahertz time-domain spectroscopy system that nitrogen is tested, obtain the time domain waveform of THz wave, as the reference signal, triplicate is averaged;
3) utilize the terahertz time-domain spectroscopy system that the pesticide specimen is tested, obtain the time domain waveform of its THz wave, as pesticide specimen signal, triplicate is averaged;
4) mean value of reference signal and the mean value of pesticide specimen signal are carried out Fourier transform respectively, obtain the Terahertz frequency domain figure of reference signal and the Terahertz frequency domain figure of pesticide specimen signal;
5) employing is extracted the absorption coefficient of pesticide specimen based on the data processing model of fresnel formula
And refractive index
,
In formula (1) and (2), be respectively the ratio and the phase differential of the amplitude of pesticide specimen signal and reference signal, its numerical value can be drawn by test; D is the thickness of pesticide specimen; C is the speed that electromagnetic wave is propagated in a vacuum;
Be frequency;
The light path of test environment: THz is filled with nitrogen, and relative humidity is less than 4.0% in the case.
2. the lossless detection method of the absorption coefficient of a kind of pesticide according to claim 1 and refractive index is characterized in that described pesticide sample is: chlorpyrifos-methyl, arprocarb and fenvalerate.
3. the lossless detection method of the absorption coefficient of a kind of pesticide according to claim 1 and refractive index is characterized in that the frequency of described chlorpyrifos-methyl
Be 0.4-1.6 THz, the frequency of arprocarb
Be 0.4-1.8 THz, the frequency of fenvalerate
Be 0.4-2.0 THz.
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| CN102207457A (en) * | 2011-04-01 | 2011-10-05 | 中国计量学院 | Method for determining optical parameters of solid bactericide pesticide |
| CN102749297A (en) * | 2012-07-10 | 2012-10-24 | 中国计量学院 | Pesticide identification method based on terahertz theoretical simulation spectrum |
| CN103196868A (en) * | 2013-04-10 | 2013-07-10 | 上海理工大学 | Determination method of refractive index of photoresist |
| CN103278474A (en) * | 2013-05-06 | 2013-09-04 | 河北大学 | Method for measuring glass refractive index |
| CN103335976A (en) * | 2013-06-04 | 2013-10-02 | 中国石油大学(北京) | Method for measuring concentrations of sulfate, nitrate solutions by utilizing terahertz time-domain spectroscopy |
| CN103424372A (en) * | 2013-08-26 | 2013-12-04 | 青岛科技大学 | Solid pesticide classification method based on decision tree algorithm |
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2010
- 2010-12-16 CN CN 201010591360 patent/CN102116739A/en active Pending
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| 《J.Opt.Soc.Am.A》 20010731 Timothy D.Dorney et al. Material parameter estimation with terahertz time-domain spectroscopy 1562-1571 1-3 第18卷, 第7期 2 * |
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| CN102207457A (en) * | 2011-04-01 | 2011-10-05 | 中国计量学院 | Method for determining optical parameters of solid bactericide pesticide |
| CN102749297A (en) * | 2012-07-10 | 2012-10-24 | 中国计量学院 | Pesticide identification method based on terahertz theoretical simulation spectrum |
| CN102749297B (en) * | 2012-07-10 | 2014-07-16 | 中国计量学院 | Pesticide identification method based on terahertz theoretical simulation spectrum |
| CN103196868A (en) * | 2013-04-10 | 2013-07-10 | 上海理工大学 | Determination method of refractive index of photoresist |
| CN103278474A (en) * | 2013-05-06 | 2013-09-04 | 河北大学 | Method for measuring glass refractive index |
| CN103278474B (en) * | 2013-05-06 | 2016-01-20 | 河北大学 | A kind of measuring method of glass refraction |
| CN103335976A (en) * | 2013-06-04 | 2013-10-02 | 中国石油大学(北京) | Method for measuring concentrations of sulfate, nitrate solutions by utilizing terahertz time-domain spectroscopy |
| CN103335976B (en) * | 2013-06-04 | 2015-12-23 | 中国石油大学(北京) | Utilize the method for terahertz time-domain spectroscopy detecting the contet of sulphate, nitrate solution concentration |
| CN104237143A (en) * | 2013-06-08 | 2014-12-24 | 青岛科技大学 | Solid pesticide identification method based on terahertz spectroscopy |
| CN103424372A (en) * | 2013-08-26 | 2013-12-04 | 青岛科技大学 | Solid pesticide classification method based on decision tree algorithm |
| CN104007115A (en) * | 2014-05-28 | 2014-08-27 | 中国石油大学(北京) | Method and system for detecting jewelry structure by using terahertz time domain spectroscopic technique |
| CN104007075A (en) * | 2014-05-28 | 2014-08-27 | 中国石油大学(北京) | Method and system for detecting crystal growth environment by using terahertz time-domain spectroscopy technology |
| CN104181122A (en) * | 2014-08-06 | 2014-12-03 | 首都师范大学 | Method for detecting content of pesticide in cereal by utilizing terahertz time-domain spectroscopy |
| CN105241840A (en) * | 2015-09-17 | 2016-01-13 | 谢文科 | Detection method for full-ingredient granules Chinese herbal medicine flos rosae chinensis based on terahertz spectrum technology |
| CN106092966A (en) * | 2016-05-27 | 2016-11-09 | 北京环境特性研究所 | A kind of choosing method of Terahertz frequency range rcs measurement timbering material |
| CN106092966B (en) * | 2016-05-27 | 2019-03-26 | 北京环境特性研究所 | A kind of choosing method of Terahertz frequency range rcs measurement timbering material |
| CN107478604A (en) * | 2017-07-10 | 2017-12-15 | 中国科学院上海光学精密机械研究所 | The measurement apparatus and measuring method of refractive index of transparent materials |
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Application publication date: 20110706 |