CN102252974A - Degenerate four-wave mixing spectroscopic technology-based method for determining historical relic producing area - Google Patents
Degenerate four-wave mixing spectroscopic technology-based method for determining historical relic producing area Download PDFInfo
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Abstract
The invention discloses a degenerate four-wave mixing spectroscopic technology-based method for determining a historical relic producing area. The method comprises the following steps of 1, dissolving a historical relic sample needing to be determined by a nitric acid solution with a concentration of 1% and transforming lead compounds in the lead-containing historical relic sample into lead atoms, 2, splitting a laser beam into three laser beams with equal light paths and adjusting space positions of the three laser beams, 3, arranging the historical relic sample needing to be determined at an intersection point of the three laser beams to obtain degenerate four-wave mixing (DFWM) signals produced by an interaction of the three laser beams and the lead atoms, 4, acquiring a DFWM signal spectrum of the lead atoms, 5, analyzing lead isotope types according to the DFWM signal spectrum to obtain a concentration ratio of lead isotopes, and 6, comparing the concentration ratio of the lead isotopes to a standard ratio of mineral aggregate lead isotopes to determine a historical relic producing area and a mineral aggregate source through analysis and deduction. The method has the advantages that a detection sensitivity of isotopes is improved; a detection limit and a sampling amount are reduced; a nondestructive detection is realized; technical equipment is simple; the operation is convenient; and an ultra-high sensitivity and a detection precision are obtained.
Description
Technical field
The invention belongs to the nonlinear optical spectral technology and use and scientific and technological archaeological technique category, relate to a kind of historical relic place of production assay method, particularly a kind of historical relic place of production measuring method based on degeneration four-wave mixing (DFWM) spectral technique.
Background technology
China is time-honored ancient civilized country, and rich and varied, precious cultural heritage is arranged, the in store very abundant historical relic in above and below ground.The distinctive spiritual value of the Chinese nation is not only being contained in these historical remnants, and is non-renewable precious resources and national crystallization of wisdom.In recent years, along with the quickening of economical globalization tendency and modernization, the cultural heritage and the living environment thereof of China are subjected to serious threat, and the research of strengthening cultural heritage is very urgent with protection.How to utilize modern science analytical approach and technological means, set up the key subjects that high precision historical relic place of production assay method has become the cultural heritage protection and repaired.
The research in the historical relic place of production and mineral aggregate source is that the science and technology archaeology is studied one of field of carrying out the earliest and coming into one's own always.Technology commonly used at present has neutron activation analysis method, inductively coupled plasma emission spectrography, plasma mass method etc., that these methods exist is low such as sensitivity and resolution, consumption sample amount is big, may be subjected to matrix effect, isobaric interference, need the deficiency of loaded down with trivial details pre-treatment, and the application that makes these methods measure in the historical relic place of production and mineral aggregate source is greatly limited.Plumbous (Pb) isotopic ratio method is a kind of emerging historical relic component detection method, and its accuracy is very high.All objects all contain lead on the earth, rock forming mineral no matter, and air, water and soil, or metalware, coin, pigment, and in the various biosome, so the scope of application of lead isotope ratioing technigue is also very wide.The lead isotope ratio of the different places of production and different mineral aggregates is different, therefore, the lead isotope ratio data of institute's working sample is compared analysis, can judge the similarities and differences in the mineral aggregate source of different samples.And data and the geological and mineral data measured are compared, just can determine its mineral aggregate place of production (Zhao Congcang, scientific and technological archaeology outline, Beijing: Higher Education Publishing House, 2006.).
Up to now, mass-spectrometric technique is the main means of isotope analysis.Yet mass-spectrometric technique has a lot of defectives, as cost height, sample pre-treatments complexity, detection length consuming time etc.The consumption sample amount of mass-spectrometric technique big (Gamma Magnitude), this drawback make it can not satisfy does not far away have the requirement that undermines nearly Non-Destructive Testing, as rare cultural relics etc.The another one critical defect of mass-spectrometric technique is that isobar disturbs, this makes a lot of isotopes not differentiated, also lower (the Dominic Lariviere of precision, Vivien F. Taylor, R. Douglas Evans, R. Jack Cornett. Spectrochimica. Acta Part B 2006,61 877.).Owing to there is not effective lead isotope ratio measurement method at present, lead isotope ratio is surveyed the method in the historical relic place of production and can't be used widely.
Summary of the invention
At defective that exists in the prior art or deficiency, the objective of the invention is to, provide a kind of based on DFWM spectral technique historical relic place of production assay method, this method can improve isotope detection sensitivity, can reduce detection limit, reduce sampling amount, realize nearly Non-Destructive Testing, and this technical equipment be simple relatively, be convenient to operation, have ultralow detection limit, hypersensitivity and accuracy of detection.
In order to achieve the above object, the present invention adopts following technical solution:
A kind of historical relic place of production assay method based on the degeneration four-wave mixing spectral technique is characterized in that: specifically carry out according to the following steps:
(1) with the salpeter solution dissolving of historical relic sample to be measured, in the high temperature atomizer, the lead compound in the historical relic sample to be measured is converted to lead atom with 1% mass concentration;
(2) beam of laser is divided into three-beam; Adjust the locus of three-beam, make the relative position of three-beam satisfy: a, equivalent optical path; In b, the three-beam two bundle travel path overlap and the direction of propagation opposite, last a branch of light and other two-beams overlap the path with greater than 0 ° and less than 1 ° angle of intersection in a bit;
(3) at the joining place of described three-beam lead atom sample to be measured is set, the common and lead atom interaction generation degeneration four-wave mixing signal of this three-beam;
(4) centre frequency of scanned laser with the degeneration four-wave mixing signal of photodetector measurement lead isotope, obtains the degeneration four-wave mixing signal spectrum with the lead atom of laser instrument centre frequency variation;
(5) analyze the kind of contained lead isotope in the historical relic sample according to the peak position of degeneration four-wave mixing signal spectrum; With the isotopic degeneration four-wave mixing signal intensity rate of different lead atoms evolution, obtain the concentration ratio between the variety classes lead isotope;
(6), analyze the place of production and the mineral aggregate source of inferring historical relic with gained lead isotope concentration ratio and the contrast of mineral aggregate lead isotope standard ratio.
The present invention also comprises following other technical characterictic:
There is lead atom energy level resonant frequency in described laser and near continuously-tuning this frequency.
Described laser linewidth is less than the lead isotope spectrum interval.
Method of the present invention is used the place of production and the mineral aggregate source that brand-new thinking is measured historical relic, promptly uses nonlinear spectroscopy commercial measurement isotope.Compare with mass-spectrometric technique, the present invention has the following advantages:
(1) simplified equipment, reduced operation easier, saved cost;
(2) empirical tests, detection limit reach the Acker magnitude; Greatly reduce detection limit, reduced sampling amount.
(3) because the DFWM signal is a coherent light, accuracy of detection is improved greatly, avoided with heavily disturbing.
(4) adopt 1/2nd wave plates to add the polarization beam splitting cube and make up beam splitting, by rotating the intensity of 1/2nd wave plates control three beams of laser, obtain maximum signal intensity, in addition, this beam split means can also be controlled the polarization state of DFWM, effectively avoid background interference, improve signal to noise ratio (S/N ratio).
Description of drawings
Fig. 1 is a light path synoptic diagram of the present invention.Wherein, each label implication is as follows:
The 1-laser instrument; 21-first total reflective mirror; 22-second total reflective mirror; 23-the 3rd total reflective mirror; 24-the 4th total reflective mirror; 25-the 5th total reflective mirror; 26-the 6th total reflective mirror; 31-the 1/1st wave plate; 32-the 1/2nd wave plate; 33-the 1/3rd wave plate; The 41-first polarization beam splitting cube; The 42-second polarization beam splitting cube; 43-the 3rd polarization beam splitting cube; 44-the 4th polarization beam splitting cube; The 5-graphite furnace atomizer; The 6-spatial light filter; The 7-photodetector.
Fig. 2 is the DFWM spectrum of lead atom.
Below in conjunction with the drawings and specific embodiments the present invention is done further and to explain.
Embodiment
Embodiment 1:
Prepare following test component:
Laser instrument is selected emitted laser centre frequency and the identical laser instrument of lead atom energy level resonant frequency for use, and laser linewidth is less than the isotopic spectrum interval of lead atom, and laser instrument can continuous tuning near the isotopic energy level resonant frequency of lead atom.Specifically select the narrow bandwidth ring dye laser or the semiconductor laser of continuously-tuning for use.
6 of identical total reflective mirrors plate 45 ° of high-reflecting films (〉 99% of this laser frequency scope to total reflective mirror according to the frequency of laser instrument emission laser).
3 of 1/2nd identical wave plates, selection is suitable for 1/2nd wave plates of laser frequency scope.
4 in identical polarization beam splitting cube, selection is suitable for the polarization beam splitting cube of laser frequency scope.
Graphite furnace atomizer.
Spatial light filter.
Photodetector; Be chosen in the photodetector of the high response of laser wavelength range.
As shown in Figure 1, the historical relic place of production assay method based on the degeneration four-wave mixing spectral technique of the present invention, specifically carry out according to the following steps:
Set a coordinate-system xyz, wherein, the xy face is defined as horizontal table top.
(1) with the salpeter solution dissolving of historical relic sample to be measured, enters the graphite furnace atomizer atom by the graphite furnace injector then and turn to the sample that contains lead atom with 1% mass concentration.
(2) laser instrument is placed A point on the horizontal table top, open laser instrument 1 output laser, this laser is the horizontal linear polarization light that the polarization direction is parallel to surface level, propagates along x axle negative sense; 2 of B on the path of this laser, C set gradually the 1/1st wave plate 31, the first polarization spectro cube 41, and described laser is normal incidence the 1/1st wave plate 31 and first polarizing cube 41 successively; The optical axis direction of the 1/1st wave plate 31 is parallel to the y axle, the angle of the cemented surface of first polarizing cube 31 and xy face is 90 °, the angle of this cemented surface and xz face is 45 °, rotate the 1/1st wave plate 31 and make its optical axis turn clockwise 35 °, become P0 light thereby described horizontal linear polarization polarisation of light direction turned clockwise 70 ° along the vertical plane at its place.Behind the first polarization spectro cube 41, become P1 light after the horizontal linear polarization component transmission of P0 light, become S1 light after the vertical curve polarized component reflection of P0 light;
2 of E on the path of S1 light, F place the 1/2nd wave plate 32, the second polarization spectro cube 42 successively, and the length of line segment CF is less than 30 centimetres; S1 light is normal incidence the 1/2nd wave plate 32 and second polarizing cube 42 successively; The optical axis direction of the 1/2nd wave plate 32 is parallel to the z axle, and the angle of the cemented surface of second polarizing cube 42 and xy face is 90 °, and the angle of this cemented surface and xz face is 45 °; Rotate the 1/2nd wave plate 32 and make its optical axis turn clockwise 22.5 °, make S1 polarisation of light direction turn clockwise 45 ° and become S2 light; Behind the second polarization spectro cube 42, become P2 light after the horizontal linear polarization component transmission of S2 light, become S4 light after the vertical curve polarized component reflection of S2 light.
D point on the P1 light path is placed first total reflective mirror 21, and the length of line segment CD is 30 centimetres, and the plated film face of first total reflective mirror 21 and the angle of xy face are 90 °, and this plated film face normal plane is negative 45 ° with respect to the xz face; P1 light is propagated along y axle negative sense through first total reflective mirror, 21 reflection backs.K point on the P1 light path is placed the 5th total reflective mirror 25, and the length of line segment DK is 50 centimetres, and the plated film face of the 5th total reflective mirror 25 and the angle of xy face are 90 °, and the normal plane of this plated film face is 45 ° with respect to the xz face; P1 light after the reflection of the 5th total reflective mirror 25 along the forward-propagating of x axle.
I point on the S4 light path is provided with the 3rd total reflective mirror 23, and the length of line segment FI is 30 centimetres, and the plated film face of the 3rd total reflective mirror 23 and the angle of xy face are 90 °, and this plated film face normal plane is negative 135 ° with respect to the xz face; S4 light is propagated along y axle negative sense after 23 reflections of the 3rd total reflective mirror;
G point on the P2 light path is provided with the 1/3rd wave plate 33, and the length of line segment CG is less than 30 centimetres, and the optical axis direction of P2 light positive incident the 1/3rd wave plate 33, the 3 1/2nd wave plates 33 is parallel to the x direction; Rotate the 1/3rd wave plate 33 and make its optical axis turn clockwise 45 °, thereby make P2 light become the S3 light of vertical curve polarization; H point on the S3 light path is placed second total reflective mirror 22, the length of line segment CH is 30 centimetres, the plated film face of second total reflective mirror 22 and the angle of xy face are 90 °, and this plated film face normal plane is 45 ° with respect to the xz face, S3 light after the reflection of second total reflective mirror 22 along the forward-propagating of x axle; J point on the S3 light path is provided with the 4th total reflective mirror 24, and the length of line segment HJ is 30.5 centimetres; The plated film face of the 4th total reflective mirror 24 and the angle of xy face are 90 °, and this plated film face normal plane is negative 135 ° with respect to the xz face; When placing the 4th total reflective mirror 24, make the 4th total reflective mirror 24 can reflect S3 light and do not stop S4 light; Along the propagation of y axle negative sense, the distance of S3 light and xy face equals the distance of S4 light and xy face to S3 light through the 4th total reflective mirror 24 reflection back, and S3 light and the distance of S4 light on the x direction are 0.5 centimetre;
L point on the path of S4 light is placed the 3rd polarization spectro cube 43, makes that S3 light also can incident the 3rd polarization spectro cube 43, and the length sum of line segment LI and line segment CF equals the length of line segment DK; The angle of the cemented surface of the 3rd polarizing cube 43 and xy face is 90 °, and the angle of this cemented surface and xz face is 45 °; Graphite furnace atomizer 5 is placed the point midway of KL.S4 light overlaps with P1 light after 43 reflections of the 3rd polarizing cube; The 4th total reflective mirror 24 that turns clockwise makes the plated film face normal plane of the 4th total reflective mirror 24 rotate in 135 ° to 136 ° scopes with respect to the angle of xz face, up to making S3 light intersect at the mid point of line segment KL through the 3rd polarizing cube 43 reflection backs and S4 light.
At this moment, the three-beam of telling from beam of laser: P1 light, S3 light and S4 light satisfy aplanatism, and P1 light is opposite with the S4 optical propagation direction, and travel path overlaps, and the angle of S3 light and S4 light is that 0.01 rad(is less than 1 °).
(3) graphite furnace atomizer 5 is placed on the mid point of line segment KL, thereby make P1 light and S3 light, S4 light intersect at the central authorities of graphite furnace atomizer 5.P1 light, S3 light and S4 light common with graphite furnace atomizer in lead atom interact generation DFWM signal.Filter P1 light with spatial light filter 6, only remain the DFWM signal; Placing the give out light cemented surface of cube 34 and the angle of xy face of the 4th polarization spectro cube 44, the 6th total reflective mirror 26, the four polarizations on the DFWM signal path after spatial light filter 6 successively is 90 °, and the angle of this cemented surface and xz face is 45 °; The plated film face of the 6th total reflective mirror 26 and the angle of xy face are 90 °, and the normal plane of this plated film face is negative 135 ° with respect to the xz face; The DFWM signal after the 6th total reflective mirror 26 reflects, is placed photodetector 7, the light-sensitive surface of DFWM signal normal incident light electric explorer 7 by the 4th polarization spectro cube 44 on the path of DFWM signal.
(4) centre frequency of scanned laser, and measure the DFWM signal of isotope sample to be measured with photodetector 7, obtain the DFWM signal spectrum that changes with the laser instrument centre frequency.
(5) analyze the kind of contained lead isotope in the historical relic sample according to the peak position of DFWM signal spectrum; With the ratio evolution of the isotopic DFWM signal intensity of different lead atoms, obtain the concentration ratio between the different lead atom isotopes;
(6) with gained lead isotope concentration ratio and the contrast of mineral aggregate lead isotope standard ratio, the place of production of analysis and judgement historical relic and mineral aggregate source.
As shown in Figure 2, use method of the present invention that plumbous (Pb) atomic sample is tested, in the step (4), 4.073 * 10
5The centre frequency of ± 2.5GHz frequency range internal scanned laser.Obtain the DFWM spectrum of lead atom, among the figure, five peaks belong to Pb-204 from left to right respectively, Pb-207, and Pb-206, Pb-207, Pb-208 this shows, method of the present invention can be differentiated the lead atom isotope, has high resolving power.
Followingly be described further according to theoretical procedure:
In like manner, the 1/2nd wave plate 32 changes in the polarization direction by polarization beam splitting cube 41 beam reflected, and its level and vertical component are by the second polarization beam splitting cube 42 separately.If horizontal component is
, establish vertical component and be
When
The time, then have
, visible DFWM signal with
The direction of propagation is opposite.
The DFWM signal that produces
Light intensity be:
（2）
（3）
Claims (3)
1. historical relic place of production assay method based on the degeneration four-wave mixing spectral technique is characterized in that: specifically carry out according to the following steps:
(1) with the salpeter solution dissolving of historical relic sample to be measured, in the high temperature atomizer, the lead compound in the historical relic sample to be measured is converted to lead atom with 1% mass concentration;
(2) beam of laser is divided into three-beam; Adjust the locus of three-beam, make the relative position of three-beam satisfy: a, equivalent optical path; In b, the three-beam two bundle travel path overlap and the direction of propagation opposite, last a branch of light and other two-beams overlap the path with greater than 0 ° and less than 1 ° angle of intersection in a bit;
(3) at the joining place of described three-beam lead atom sample to be measured is set, the common and lead atom interaction generation degeneration four-wave mixing signal of this three-beam;
(4) centre frequency of scanned laser with the degeneration four-wave mixing signal of photodetector measurement lead isotope, obtains the degeneration four-wave mixing signal spectrum with the lead atom of laser instrument centre frequency variation;
(5) analyze the kind of contained lead isotope in the historical relic sample according to the peak position of degeneration four-wave mixing signal spectrum; With the isotopic degeneration four-wave mixing signal intensity rate of different lead atoms evolution, obtain the concentration ratio between the variety classes lead isotope;
(6), analyze the place of production and the mineral aggregate source of inferring historical relic with gained lead isotope concentration ratio and the contrast of mineral aggregate lead isotope standard ratio.
2. according to claims 1 described method, it is characterized in that: there is lead atom energy level resonant frequency in described laser and near continuously-tuning this frequency.
3. according to claims 1 described method, it is characterized in that: described laser linewidth is less than the lead isotope spectrum interval.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104101570A (en) * | 2014-05-06 | 2014-10-15 | 浙江省海洋开发研究院 | Hairtail producing area detection method by infrared spectroscopy |
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| CN101393373A (en) * | 2007-09-21 | 2009-03-25 | 哈尔滨工业大学 | Self-stable light splitting technology for four wave mixing experiment |
| JP2010164351A (en) * | 2009-01-14 | 2010-07-29 | Kowa Co | Optical tomographic imaging apparatus |
| CN101968434A (en) * | 2010-09-26 | 2011-02-09 | 西北大学 | DFWM (Degenerate Four-Wave Mixing) spectroscopic technology based method for determining date of cultural relics |
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Patent Citations (3)
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|---|---|---|---|---|
| CN101393373A (en) * | 2007-09-21 | 2009-03-25 | 哈尔滨工业大学 | Self-stable light splitting technology for four wave mixing experiment |
| JP2010164351A (en) * | 2009-01-14 | 2010-07-29 | Kowa Co | Optical tomographic imaging apparatus |
| CN101968434A (en) * | 2010-09-26 | 2011-02-09 | 西北大学 | DFWM (Degenerate Four-Wave Mixing) spectroscopic technology based method for determining date of cultural relics |
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| 贾腊江等: "混频激光光谱分析技术在文化遗产研究中的应用前瞻", 《西北大学学报(哲学社会科学版)》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104101570A (en) * | 2014-05-06 | 2014-10-15 | 浙江省海洋开发研究院 | Hairtail producing area detection method by infrared spectroscopy |
| CN104101570B (en) * | 2014-05-06 | 2016-05-11 | 浙江省海洋开发研究院 | A kind of infra-red sepectrometry detects the method in the hairtail place of production |
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