CN112378890A - Method for judging amber production area based on phosphorescence lifetime - Google Patents
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Abstract
The invention discloses a method for judging amber production area based on phosphorescence lifetime, belonging to the technical field of jewelry identification. The method comprises the following steps: detecting the phosphorescence lifetime of amber; the amber origin was determined from the phosphorescence lifetime. The invention relates to a method for judging amber production areas based on phosphorescence lifetime, which is characterized in that firstly, based on the different properties of phosphorescence lifetime of amber in different production areas, the amber production areas are distinguished and judged through the phosphorescence lifetime, and a new means is provided for amber identification work; secondly, the amber is irradiated by a low-power excitation source, so that the damage to the amber in the judging process is avoided; thirdly, the detection is carried out by adopting a multi-time excitation-recording mode, so that the accuracy of the detection result is improved; fourthly, an exponential decay fitting function with three life terms is adopted, and a more accurate amber phosphorescence life value can be obtained; fifthly, corresponding values of amber phosphorescence lifetimes of different producing areas are given and used as a reference for judging the amber producing areas.
Description
Technical Field
The invention belongs to the technical field of jewelry identification, and particularly relates to a method for judging an amber production area based on phosphorescence lifetime.
Background
Amber is natural petrochemical resin formed by liquid resin of gymnosperm (Pinaceae, Najaceae, Pinaceae) or angiosperm (Leguminosae, Dipterocarpaceae) after multiple geological actions, and is mixture of macromolecular organic substances. The age of formation of amber is large, with the common species coming from the middle chalk age to the ancient-recent age of the new age, and the minority species coming from the triassic and Jurassic ages, even going back to the stone charcoal age (320 Ma). In recent years, the amber appearing in the international jewelry market is mainly burma amber, baltic sea amber, mexico amber and dominican amber. Of the ambers in different producing areas, the body color of the ambar amber is mainly golden brown-brownish red, and the body color of the ambar amber is a few green (willow green), and the ambar amber has unique color and special optical effects (such as chameleon and violet). The body color of the boswellia succinum is mainly yellow-reddish brown, and the boswellia succinum is bright in color and has various internal characteristics (such as beeswax, white wax, amber and the like), so that the boswellia succinum is favored by Chinese consumers in recent years. Most of Mexico amber and Dorniaga amber have mysterious blue-green fluorescence, the blue-green fluorescence is probably related to the content of a compound Perylene, and blue amber with higher quality is short of demand due to the rare yield.
The judgment of the origin of amber is one of the works in the field of jewelry identification. In the prior art, a method for judging the production place of amber by a plurality of technical means such as infrared spectrum, Raman spectrum, nuclear magnetic resonance spectrum and the like exists. The infrared spectrum can only carry out single-piece detection on amber samples, can not detect a large number of samples in different batches, and has low efficiency for the purpose of identifying and distinguishing the production places. The infrared spectrum testing method related to amber is mainly divided into two methods of reflection method and powder transmission method, and the sample red obtained by reflection methodThe interference of noise signals of an external spectrogram is large, K-K conversion is needed, and an infrared spectrogram of a sample obtained by a powder transmission method is a destructive testing method and is not suitable for amber, a medium-high grade precious stone. Raman spectroscopy and13the C nuclear magnetic resonance also needs to damage the amber in a small range, and the damage test is destructive and long in test time. Since the amber of different producing areas usually has partially same or similar characteristics, if the judgment is made by observing the appearance of the amber only through personal experience, the judgment result not only lacks objectivity and persuasion, but also is easy to generate misjudgment.
The amber is classified according to the producing area, mainly including Burma amber, Bordea sea amber, Mexico amber and dominican amber, and the amber of different producing areas also has subclasses. For example, Burma amber is divided into black tea amber, golden blue amber, violet amber and chameleon amber according to color. Jiangxiang et al author in the paper of the special optical effect of Burma amber, proposed that Burma amber has a phosphorescent effect, and studied that different luminescence centers of different species of Burma amber (black tea amber, green tea amber, discolored Dragon amber and golden amber) show different phosphorescent lifetimes. However, since the phosphorescence lifetimes of different luminescence centers of the same sample are different, and the test results thereof are influenced by a plurality of experimental conditions, such as the size, thickness, excitation light source intensity, and irradiation time of the amber sample, and a series of dynamic difference values are presented, the research only indicates that the luminescence behaviors of different luminescence centers of the same amber sample are different, and cannot solve the technical problem of determining the amber production place according to the average phosphorescence lifetime, which is to be solved by the present invention, and therefore, a large-batch, rapid, and lossless determination method for accurately identifying the amber production place is urgently needed in the technical field of jewelry identification.
Disclosure of Invention
In order to solve the problems encountered in the technical field of jewelry identification, the invention provides a method for judging an amber production area based on phosphorescence lifetime, which comprises the following steps:
step 10: detecting the phosphorescence lifetime of amber;
step 20: the amber origin was determined from the phosphorescence lifetime.
Further, the method for detecting the phosphorescence lifetime of amber in step 10 specifically includes:
step 101: irradiating the amber through an excitation light source, and recording the generation rate of phosphorescence photons generated by the excited amber;
step 102: establishing a time-resolved fluorescence/phosphorescence spectrogram according to the irradiation time and the phosphorescence photon generation rate;
step 103: fitting the images of the time-resolved fluorescence/phosphorescence spectrograms to an exponential decay fitting function;
step 104: and obtaining the amber phosphorescence lifetime value according to the exponential decay fitting function.
In step 101, the excitation light source is an ultraviolet light source with power of 200 and 500 microwatts per square centimeter; further, in step 101, the excitation light source is an ultraviolet light source with a power of 300 microwatts per square centimeter.
The wavelength of the ultraviolet light source in the step 101 is 353-373 nm; further, the wavelength of the ultraviolet light source in step 101 is 365 nm.
In step 101, a multiple "excitation-recording" method is used for detection, which includes:
step 1011: irradiating amber by an exciting light source for a period of time t1；
Step 1012: irradiation time t1After finishing, closing the excitation light source; detecting phosphorescence photons generated by amber excitation through a photoreceptor, and recording the generation rate of the phosphorescence photons, wherein the recording time is t2；
Step 1013: recording the time t2After the end, t is determined2Whether a peak in the phosphorescent photon generation rate recorded over time reaches a first threshold; if yes, end step 101; if not, return to step 1011 to perform the next "fire-record" process.
Further, the irradiation time period t12-5 seconds, said recording time period t23-8 seconds, and the first threshold value is 1000-3000.
Further, step 103The exponential decay fitting function is an exponential decay fitting function with three life terms, and the expression of the exponential decay fitting function is as follows: y is(t)＝A+B1e(-t/T1)+B2e(-t/T2)+B3e(-t/T3) Wherein t is a time variable; a, B1、B2、B3，T1、T2、T3Is a constant.
Further, the reference for determining the amber production area according to the phosphorescence lifetime in the step 20 is as follows: if the phosphorescence lifetime falls within the interval of 0.32370 s-0.53880 s, judging the amber as Burma amber; if the phosphorescence lifetime falls within the interval 0.00560 s-0.01431 s, determining that the amber is the Porosira amber; if the phosphorescence lifetime falls within the interval 0.06352 s-0.29090 s, determining that the amber is Mexico amber; if the phosphorescence lifetime falls within the interval 0.02113 s-0.04092 s, the amber is determined to be dominican amber.
The invention has the beneficial effects that:
1. the method for judging the amber production area based on the phosphorescence service life is strong in objectivity and high in accuracy of detection results, and is large in batch and rapid.
2. The invention relates to a method for judging amber production places based on phosphorescence lifetime, which is characterized in that based on the different properties of phosphorescence lifetime of amber in different production places, the amber production places are distinguished and judged through the phosphorescence lifetime, and the method does not make the same requirement on the size of an amber sample, the amber samples in different production places can be in irregular shapes with different sizes, and the finally obtained phosphorescence lifetime value cannot be influenced by the intensity and the irradiation time of an excitation light source, thereby providing a new means for amber judgment work;
3. the amber is irradiated by a low-power excitation source, so that the damage to the amber in the judging process is avoided;
4. the detection is carried out by adopting a multi-time excitation-recording mode, so that the accuracy of the detection result is improved;
5. by adopting an exponential decay fitting function with three life terms, a more accurate amber phosphorescence life value can be obtained;
6. corresponding values of amber phosphorescence lifetime in different producing areas are given as a reference for amber producing area judgment.
7. The method can be used for simultaneously detecting the phosphorescence life of a plurality of amber samples, not only further reduces the experimental error under the same experimental conditions and enables the measurement precision to be more accurate, but also provides a new technical scheme for batch judgment of amber production areas, saves the judgment time and better accords with the concept of cost economy.
Drawings
FIG. 1 is a schematic view showing the overall flow of a method for determining an amber production area based on phosphorescent lifetime in example 1;
FIG. 2 is a schematic overall flow chart for detecting the phosphorescence lifetime of amber in example 1;
FIG. 3 is a schematic overall flow chart of example 1, in which amber is irradiated by an excitation light source, and the generation rate of phosphorescence photons generated by the excited amber is recorded;
FIG. 4 is a time-resolved fluorescence/phosphorescence spectrum generated in example 2.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
amber photoluminescence includes both fluorescence and phosphorescence. Fluorescence is a light quantum emitted when electrons jump from the lowest vibration level of the first excited state singlet state to any vibration level of the ground state singlet state, and fluorescence disappears immediately after irradiation of exciting light stops; and phosphorescence is a light quantum emitted by the transition from the lowest vibrational level of the first electronic excited state triplet state to any vibrational level of the ground state singlet state, and the phosphorescence continues for a while after the excitation light stops irradiating. The phosphorescence energy is smaller than the fluorescence, the wavelength is longer than the fluorescence, and the phosphorescence lifetime is longer than the fluorescence lifetime. Burma, Polaroid, Mexico and dominican amber have special phosphorescence. When amber is irradiated by incident light (usually ultraviolet light or X-ray) of a certain wavelength, the light energy is absorbed and enters an excited state (usually with a spin multiplicities different from the ground state), and then slowly excites and emits outgoing light (usually with a wavelength in the visible band) longer than the wavelength of the incident light, and when the incident light stops, the light emission phenomenon continues.
The phosphorescence lifetime represents the property of the amber, and is not influenced by the size, thickness and wavelength and intensity of an excitation light source, and the phosphorescence lifetime of the amber in different production places is greatly different due to the large difference of ancient plant sources, main chemical components, formation age and burying environment. Therefore, for amber (including amber raw stone and processed amber artware) with unknown production place, the production place can be distinguished by utilizing the phosphorescence lifetime of the amber.
Example 1:
the embodiment provides a method for judging amber production area based on phosphorescence lifetime, which comprises the following steps as shown in FIG. 1:
step 10: detecting the phosphorescence lifetime of amber;
step 20: the amber origin was determined from the phosphorescence lifetime.
The method for detecting the phosphorescence lifetime of amber in step 10 is shown in fig. 2, and comprises the following steps:
step 101: irradiating the amber through an excitation light source, and recording the generation rate of phosphorescence photons generated by the excited amber;
preferably, the excitation light source is an ultraviolet light source with a power of 200-; specifically, the excitation light source is a laser ultraviolet light source with a power of 300 microwatts per square centimeter. Because amber is different from other inorganic ores and is of an organic matter mixture structure, strong light irradiation, particularly ultraviolet light with higher energy, can cause irreversible damage to amber after long-time irradiation. For example, the full spectrum radiant power in the one square centimeter range under sunlight at noon in summer is greater than 160 milliwatts, with ultraviolet intensity greater than 4000 microwatts; while the intensity of ultraviolet light under the shade of tree is about 800 microwatts and about 200 microwatts in cloudy days. If the amber is worn in the sun for a long time, the amber can have the light aging phenomena of darkening color, darkening luster, amber body cracks and the like. Therefore, a lower power excitation light source is used in the present invention to avoid damage to the amber. Meanwhile, the power of the excitation light source is not too low, so that the detection accuracy is prevented from being reduced or the detection time is prevented from being too long.
Preferably, the wavelength selection range of the ultraviolet light source is 353-373nm, and a better detection effect can be obtained in the range; more preferably, the wavelength of the ultraviolet light source is 365 nm. The ultraviolet ray is an electromagnetic wave with the wavelength of 10-400 nm and is positioned between visible light and X-rays. In the work of detecting gemstones, the fact that whether gemstones have phosphorescence or fluorescence is tested by using 253.7nm short-wave ultraviolet light and 365nm long-wave ultraviolet light. The 253.7nm short-wave ultraviolet has higher energy, and the sample is easy to damage after being irradiated for a long time, and the sample can damage the body of an operator, so that the skin aging can be caused by the light person, and the skin cancer, the cataract and the like can be caused by the serious person, therefore, the ultraviolet is not suitable for being used in the invention. According to the study on the three-dimensional fluorescence spectrum characteristics of the amber in different producing areas, the number and the positions of fluorescence signals of amber samples in different producing areas in the three-dimensional fluorescence spectrum are different, and the wavelengths of the optimal excitation light sources are also different. Analysis of three-dimensional fluorescence spectrograms shows that Burma, Polarosea, Mexico and dominican amber have strong fluorescence peaks when the wavelength of the excitation light is in the range of 353-373nm, and therefore 365nm is preferably adopted as the phosphorescence life of the amber to be tested in order to obtain the best phosphorescence effect.
Step 102: establishing a time-resolved fluorescence/phosphorescence spectrogram according to the irradiation time and the phosphorescence photon generation rate; specifically, the abscissa of the coordinate system is the time recorded in step 101, and the zero point of the abscissa is the recording time t2Starting point of (recording time t)2See below); the longitudinal axis of the coordinate system is the photon generation rate measured in step 101; discrete points in the image constitute a function image approximating exponential decay.
Step 103: fitting the images of the time-resolved fluorescence/phosphorescence spectrograms to an exponential decay fitting function;
preferably, in step 103, the exponential decay fitting function is an exponential decay fitting having three lifetime termsA function, whose expression is: y is(t)＝A+B1e(-t/T1)+B2e(-t/T2)+B3e(-t/T3) Wherein t is a time variable; a, B1、B2、B3，T1、T2、T3Is constant and is obtained by means of fitting calculation. Generally, the exponential decay fitting function has a plurality of expression forms, and the more the life term is, the higher the accuracy of the function image fitting is, but the more the calculation amount is. In the embodiment, the exponential decay fitting function with three life terms is selected, so that a more accurate measurement result can be obtained on the premise of not increasing the calculated amount remarkably, and the judgment requirement is met. In a specific implementation, the constants can be generated by the spectral measurement device through the attached software automatically by means of fitting a roll integral calculation. Some existing spectrometers already have the above-mentioned functions, such as FLS980 steady state transient fluorescence spectrometer, Fluorolog-3 spectrometer, etc.
Step 104: and obtaining the amber phosphorescence lifetime according to the exponential decay fitting function. The phosphorescence lifetime is also automatically calculated by the spectroscopic measurement device.
In step 101, since a low-power ultraviolet light source is used as an excitation light source, the measurement accuracy is necessarily inferior to that of the high-power excitation light source. To overcome this problem, the detection is preferably performed in multiple "excitation-recording" modes in step 101, as shown in fig. 3, and includes:
step 1011: irradiating amber by an exciting light source for a period of time t1(ii) a Preferably, the irradiation time period t12-5 seconds;
step 1012: irradiation time t1After finishing, closing the excitation light source; detecting phosphorescence photons generated by amber excitation through a photoreceptor, and recording the generation rate of the phosphorescence photons, wherein the recording time is t2(ii) a Preferably, the recording time period t23-8 seconds; specifically, the recording of the phosphorescent photon generation rate refers to recording of the phosphorescence from t2Starting time to t2End time, number of phosphorescent photons detected per unit time (e.g., 1 millisecond);it is apparent that the phosphorescent photon generation rate is at t2The starting moment has the highest value (peak) and then gradually decreases.
Step 1013: recording the time t2After the end, t is determined2Whether a peak in the phosphorescent photon generation rate recorded over time reaches a first threshold; if yes, end step 101; if not, returning to the step 1011 to perform the next "excitation-recording" process; preferably, the first threshold is 1000-3000.
Specifically, in step 101, since recording is performed after the excitation light source needs to be turned off, it is preferable to use a laser light source. The laser light source has higher closing speed, and can avoid measurement interference caused by slow closing speed of the traditional xenon lamp.
The reason for this is that multiple "firing-recording" is used: to avoid damage to amber, it is preferable to use a low power excitation light source, and this approach will result in a significant reduction in measurement accuracy. Adopts the technical scheme of multiple times of excitation-recording, and t is irradiated every time1During the time, the amber absorbs the energy provided by the irradiation light source; at a subsequent t2The absorbed energy is not completely released over time, so that in subsequent times t2Over time, amber accumulates more and more energy and thus releases more and more phosphorescent photons until the first threshold is reached. At this time, the data recorded by the spectrum measuring device are accumulated, so that the phosphorescence life of the amber can be calculated more accurately. At a specific setting t1、t2And specific values for the first threshold, it should be recognized that t1The larger, t2The smaller the first threshold value is, the larger the first threshold value is, the longer the detection time is, and the more accurate the measurement result is; and vice versa. Preferably, step 101 may be repeated multiple times to obtain more measurement data, which is used as a basis for calculating the lifetime of amber phosphorescence, and the measurement accuracy may be further improved.
The criteria for determining the amber production area according to the phosphorescence lifetime in the step 20 are as follows:
if the phosphorescence lifetime falls within the interval of 0.32370 s-0.53880 s, judging the amber as Burma amber; if the phosphorescence lifetime falls within the interval 0.00560 s-0.01431 s, determining that the amber is the Porosira amber; if the phosphorescence lifetime falls within the interval 0.06352 s-0.29090 s, determining that the amber is Mexico amber; if the phosphorescence lifetime falls within the interval 0.02113 s-0.04092 s, the amber is determined to be dominican amber.
Specifically, the above-mentioned interval includes end points. The understanding of the decision result should be: and if the detected amber phosphorescence lifetime falls into a certain interval, the origin of the amber is considered as the origin corresponding to the interval. Because jewelry identification is a very complex interdisciplinary discipline, when the technical scheme provided by the invention is practically applied, other existing detection methods should be sufficiently combined when complex samples are encountered so as to obtain a more accurate judgment result.
Example 2:
this example shows a specific implementation of the method described in example 1 for identification of the origin of an amber sample.
8 amber samples to be detected with the size of 3-5 cm in length, 3-4 cm in width and 1.5 cm in thickness; the amber sample appeared yellow to tan in appearance, transparent in texture, glossy in resin appearance, etc.
The device integrates Origin software and has the functions of generating and displaying a time-resolved fluorescence/phosphorescence spectrogram, fitting an exponential decay function, calculating phosphorescence lifetime and the like.
The excitation light source is a 365nm ultraviolet band laser light source, the laser emission power is 300 microwatts, the distance between a laser head and the amber sample to be detected is about 5 cm, laser is vertically irradiated from top to bottom, and a circular light spot with the area of about 1 square cm is formed on the upper surface of the amber sample.
The assay was performed as described in example 1. Wherein, the irradiation time t in step 10113 seconds, recording time period t2At 4 seconds, the first threshold value is 2000.
Time resolved fluorescence/phosphorescence spectra were generated for 8 samples by a Fluorolog-3 spectrometer. As shown in fig. 4, 8 dotted curves are shown, indicating that the 8 samples have different phosphorescence excitation properties under the same detection conditions.
The 8 dotted curves were fitted by a Fluorolog-3 spectrometer and the phosphorescence lifetime of each sample was calculated.
As shown in the above data, the fitting results are exponential decay fitting functions of a certain curve in time-resolved fluorescence/phosphorescence spectra, wherein parameters A, B are given1、B2、B3，T1、T2、T3And a specific value of phosphorescence lifetime (AverageLifeTime).
According to the phosphorescence lifetime, the corresponding amber sample producing area can be judged. Specifically, the phosphorescence lifetime of the amber sample corresponding to the fitting result is 0.2908613s, and the amber sample falls into the interval of 0.06352-0.29090 s, and the origin of the amber sample is determined to be Mexico.
Claims (10)
1. A method for judging amber production area based on phosphorescence lifetime is characterized in that: the method comprises the following steps:
step 10: detecting the phosphorescence lifetime of amber;
step 20: the amber origin was determined from the phosphorescence lifetime.
2. The method of determining amber origins based on phosphorescence lifetime according to claim 1, wherein: the step 10 of detecting the phosphorescence lifetime of amber comprises the following steps:
step 101: irradiating the amber through an excitation light source, and recording the generation rate of phosphorescence photons generated by the excited amber;
step 102: establishing a time-resolved fluorescence/phosphorescence spectrogram according to the irradiation time and the phosphorescence photon generation rate;
step 103: fitting the images of the time-resolved fluorescence/phosphorescence spectrograms to an exponential decay fitting function;
step 104: and obtaining the amber phosphorescence lifetime according to the exponential decay fitting function.
3. The method of determining amber origins based on phosphorescence lifetime according to claim 2, wherein: in step 101, the excitation light source is an ultraviolet light source with a power of 200 and 500 microwatts per square centimeter.
4. The method of determining amber origins based on phosphorescence lifetime according to claim 3, wherein: in step 101, the excitation light source is an ultraviolet light source with a power of 300 microwatts per square centimeter.
5. The method of determining amber origins based on phosphorescence lifetime according to claim 2, wherein: the wavelength of the ultraviolet light source in step 101 is 353-373 nm.
6. The method of determining amber origins based on phosphorescence lifetime according to claim 5, wherein: in step 101, the wavelength of the ultraviolet light source is 365 nm.
7. The method of determining amber origins based on phosphorescence lifetime according to claim 2, wherein: the step 101 is performed in an "excitation-recording" manner, and includes:
step 1011: irradiating amber by an exciting light source for a period of time t1；
Step 1012: irradiation time t1After finishing, closing the excitation light source; detecting phosphorescence photons generated by amber excitation through a photoreceptor, and recording the generation rate of the phosphorescence photons, wherein the recording time is t2；
Step 1013: recording the time t2After the end, t is determined2Whether a peak in the phosphorescent photon generation rate recorded over time reaches a first threshold; if yes, end step 101; if not, return to step 1011 and repeat the "fire-record" process.
8. The method of claim 7 for determining amber origin based on phosphorescence lifetimeCharacterized in that: the irradiation time period t12-5 seconds, said recording time period t23-8 seconds, and the first threshold value is 1000-3000.
9. The method of determining amber origins based on phosphorescence lifetime according to claim 2, wherein: the expression of the exponential decay fitting function in step 103 is:
wherein t is a time variable; a, B1、B2、B3，T1、T2、T3Is a constant.
10. The method of determining amber origins based on phosphorescence lifetime according to claim 1, wherein: the criteria for determining the amber production area according to the phosphorescence lifetime in the step 20 are as follows:
if the phosphorescence lifetime falls within the interval 0.00560 s-0.01431 s, determining that the amber is the Porosira amber;
if the phosphorescence lifetime falls within the interval 0.02113 s-0.04092 s, determining that the amber is the dominican amber;
if the phosphorescence lifetime falls within the interval 0.06352 s-0.29090 s, determining that the amber is Mexico amber;
if the phosphorescence lifetime falls within the interval 0.32370 s-0.53880 s, the amber is determined to be Myanmar amber.
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