CN113376137A - Method for nondestructively identifying filling treatment of andalusite - Google Patents
Method for nondestructively identifying filling treatment of andalusite Download PDFInfo
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- CN113376137A CN113376137A CN202110768507.1A CN202110768507A CN113376137A CN 113376137 A CN113376137 A CN 113376137A CN 202110768507 A CN202110768507 A CN 202110768507A CN 113376137 A CN113376137 A CN 113376137A
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- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a method for nondestructively identifying filling treatment of andalusite, which comprises the following steps: the method comprises the following steps: selecting a andalusite sample; step two: measuring by adopting an FP-8500 fluorescence spectrometer of JASCO; step three: and (4) processing data, and comparing the fluorescence spectrum to accurately identify the andalusite. The high sensitivity of the fluorescence spectrometer can quantify the fluorescence which can not be seen through the ultraviolet fluorescent lamp, and the continuous excitation light source irradiation of the fluorescence spectrometer can completely show the fluorescence intensity distribution of the gem in the whole excitation wave band. The relative intensity of the fluorescence center of the packed andalusite is far stronger than that of the natural andalusite, so that whether the andalusite is subjected to packing treatment can be judged by analyzing the position and the relative intensity of the fluorescence center of a three-dimensional fluorescence spectrum of the andalusite. Therefore, the fluorescence spectrum analysis has obvious effect on distinguishing the natural andalusite from the filling treatment andalusite, and can be used as a method for nondestructively identifying the filling treatment andalusite.
Description
Technical Field
The invention relates to the technical field of andalusite identification, in particular to a method for nondestructively identifying, filling and processing andalusite.
Background
The andalusite minerals are rich and colorful, and the gems are various. Among them, blue-cyan andalusite is called sapphire, pink andalusite is called morgan, and sapphire and morgan are common gemstone subspecies in andalusite, and are popularized in the market with fresh color tone, high hardness and parent price, and are more and more popular and sought after by consumers in recent years along with the design favor of first-line jewelry brands. Because of the comparative development of cracks of part of the sapphire and the morgan stone, in order to meet the purchase demand of consumers, the limited andalusite stone resource needs to be fully utilized by improving the cleanliness of the sapphire and the morgan stone through optimization treatment. With the rising demand of the andalusite, the market share of the andalusite filled in the Chinese market is continuously increased, the appearance characteristics of the filled andalusite are less and less obvious, and further research on a nondestructive identification method of the filled andalusite is urgent.
The prior art is relatively sufficient to research the most expensive variety of emerald in the family of andalusite, and relates to the identification of the content, filling treatment and synthesis of the emerald and the like. The filling treatment research of the sapphire, the moore stone and the green andalusite is weak, the conventional jewel characteristics such as bubbles in sample cracks, the flowing structure of fillers and the flash effect are observed through a gem microscope at present, and the infrared absorption of organic matters is observed through a Fourier transform infrared spectrometer, so that whether the gem is filled or not is judged. Generally, the identification of the filled sapphire has certain research results, but the detection method is single and the identification of the filling treatment of other varieties of andalusite is not involved, so that the improvement is made, and a method for nondestructively identifying the filling treatment of the andalusite is provided.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a method for nondestructively identifying filling treatment of andalusite, which comprises the following steps of:
the method comprises the following steps: selecting a andalusite sample;
step two: measuring by adopting an FP-8500 fluorescence spectrometer of JASCO;
step three: and (4) processing data, and comparing the fluorescence spectrum to accurately identify the andalusite.
As a preferred technical scheme of the invention, in the step one, the andalusite sample to be detected is selected without sample preparation.
In the second step, the fluorescence spectrometer has an Emission test mode and a Manual sensitivity, wherein the PMT voltage of the sample BT-7 is 600V, the rest samples are 700V, the wavelength range of an excitation light source is 305-550 nm, and the slit width is 5 nm; the emission wavelength range is 325-650 nm, the slit width is 2.5nm, the data interval is 1nm, and the scanning speed is 2000 nm/min.
As a preferred technical scheme of the invention, in the third step, data processing is carried out, the relative intensity of the fluorescence center of the filled andalusite is obviously stronger than that of the natural andalusite, the andalusite can be accurately identified by comparing the relative intensity of the three-dimensional fluorescence spectrum, the fluorescence which cannot be seen through an ultraviolet fluorescent lamp can be quantified by the high sensitivity of the fluorescence spectrometer, and the fluorescence intensity distribution of the gem in the whole excitation waveband can be completely shown by the irradiation of a continuous excitation light source of the fluorescence spectrometer.
The invention has the beneficial effects that: in the method for nondestructively identifying and filling the andalusite, the mechanism of fluorescence generation is that after molecules of a substance absorb the energy of irradiation light, the molecules in the lowest energy level of a ground state are excited to various vibration energy levels of an electronic excited state. The excited molecules collide with surrounding molecules, and the energy is transferred and then falls to the lowest vibrational level of the excited state of the electron, whereby the vibrational level transitions to the ground state vibrational level, releasing energy in the form of fluorescence. The emitted fluorescence usually contains only one emission band, and different substances have characteristic fluorescence excitation and emission spectra, so that the qualitative analysis of the substances can be performed by using the difference of the fluorescence excitation and the emission spectra. The fluorescence spectrometer uses this principle to determine the change in intensity of the fluorescence emitted by the material under the irradiation of excitation light of successive wavelengths, in order to analyze the fluorescence characteristics of the gemstone mineral, the relative intensity of the fluorescence centre of the packed andalusite being significantly higher than that of the natural andalusite, due to the aromatic compounds in the organic glue added during the packing process. Fluorescence spectrum analysis is an effective and rapid nondestructive testing means for distinguishing natural and filling-processed andalusite.
The high sensitivity of the fluorescence spectrometer can quantify the fluorescence which can not be seen through the ultraviolet fluorescent lamp, and the continuous excitation light source irradiation of the fluorescence spectrometer can completely show the fluorescence intensity distribution of the gem in the whole excitation wave band. The relative intensity of the fluorescence center of the packed andalusite is far stronger than that of the natural andalusite, so that whether the andalusite is subjected to packing treatment can be judged by analyzing the position and the relative intensity of the fluorescence center of a three-dimensional fluorescence spectrum of the andalusite. Therefore, the fluorescence spectrum analysis has obvious effect on distinguishing the natural andalusite from the filling treatment andalusite, and can be used as a method for nondestructively identifying the filling treatment andalusite.
Drawings
FIG. 1 is a flow chart of the method of lossless discrimination packing treatment of andalusite according to the invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example (b): as shown in FIG. 1, the method for nondestructively identifying packing-treated andalusite of the invention comprises the following steps:
the method comprises the following steps: selecting a andalusite sample;
step two: measuring by adopting an FP-8500 fluorescence spectrometer of JASCO;
step three: and (4) processing data, and comparing the fluorescence spectrum to accurately identify the andalusite.
As a preferred technical scheme of the invention, in the step one, the andalusite sample to be detected is selected without sample preparation.
In the second step, the fluorescence spectrometer has an Emission test mode and a Manual sensitivity, wherein the PMT voltage of the sample BT-7 is 600V, the rest samples are 700V, the wavelength range of an excitation light source is 305-550 nm, and the slit width is 5 nm; the emission wavelength range is 325-650 nm, the slit width is 2.5nm, the data interval is 1nm, and the scanning speed is 2000 nm/min.
As a preferred technical scheme of the invention, in the third step, data processing is carried out, the relative intensity of the fluorescence center of the filled andalusite is obviously stronger than that of the natural andalusite, the andalusite can be accurately identified by comparing the relative intensity of the three-dimensional fluorescence spectrum, the fluorescence which cannot be seen through an ultraviolet fluorescent lamp can be quantified by the high sensitivity of the fluorescence spectrometer, and the fluorescence intensity distribution of the gem in the whole excitation waveband can be completely shown by the irradiation of a continuous excitation light source of the fluorescence spectrometer.
Selecting 17 green pillared stone samples, wherein two natural blue green pillaries (BN-1, BN-2), two natural pink green pillaries (BN-3, BN-4), two natural green pillaries (BN-5, BN-6), four packed pink green pillaries (BT-1, BT-2, BT-3, BT-4), four packed blue green pillaries (BT-5, BT-6, BT-7, BT-8), two packed green pillaries (BT-9, BT-10) and one heavily packed blue green pillaries (TYP), respectively performing conventional test, determination by a ThermoFisher EDX-7000 energy dispersive X-ray fluorescence analysis device, determination by Raman spectroscopy by a Bruker Senterra laser Raman spectrometer, determination by a Bruker TEX80 Fourier transform infrared spectrometer and determination by a SCO FP-8500 fluorescence spectrometer, the test results are as follows;
the natural attapulgite refractive index of the sample is between 1.57 and 1.59, and the packing-treated attapulgite refractive index is between 1.56 and 1.57, which is slightly lower than the natural attapulgite refractive index, and is probably related to the packed low refractive index adhesive. Referring to the previous research that the relative density of the natural andalusite is 2.67-2.90, the relative density of the sample is measured by hydrostatic weighing, and the relative densities of the other samples except the TYP sample are in a normal range. The relative density of the pink andalusite is slightly higher than that of the blue andalusite, the relative density of the natural andalusite and the filling-treated andalusite in the same hue has no obvious difference, and the relative density of the andalusite sample TYP subjected to the severe filling treatment is 2.582 and is lower than the normal range, so that the relative density of the andalusite subjected to the severe filling treatment is reduced due to the influence of the filling materials. The fluorescence characteristics of the sample are observed under an ultraviolet fluorescent lamp, the natural green pillared stone is inert under both long wave and short wave, the filled pink green pillstone emits weak-medium white fluorescence under both long wave and short wave according to different filling degrees, the filled blue green pillstone and the filled green pillstone emit weak-medium white fluorescence under long wave, the blue green pillstone and the filled green pillstone do not emit light under short wave, and the visible fluorescence of individual samples is distributed along cracks. Therefore, the ultraviolet fluorescent lamp can be used as a conventional auxiliary means for distinguishing the natural andalusite from the filling treatment andalusite, and the surface characteristics observed by naked eyes or microscope amplification can only be used as an auxiliary means for identifying the filling treatment andalusite;
energy dispersive X-ray fluorescence spectroscopy, natural and filled siteThe chemical elements contained in the mullite are consistent, and all samples contain Si and Al. The pink andalusite contains a certain amount of Rb and Cs and alkali metal ion Rb+、Cs+Into structural channels to balance Mn2+Substituted Al3+The electrovalence difference generated by occupying the octahedral sites. The blue and green andalusite both contain a certain amount of Fe and Fe2+And Fe3+Substitution of isomorphism for Al in Al-O octahedron3+While Fe exists in the hexagonal ring structure channel2+Hydrated ions formed with channel water and Fe3+Hydrolysis reaction with water molecular ligand in channel to generate relatively stable Fe2(OH)4]2+Multiple polymeric ions, blue and green of the andalusite being Fe2+And Fe3+The result of the combined action. Besides, the blue and green andalusite also contains a small amount of Cs, Tb and Dy, wherein the content of Cs is obviously less than that of pink andalusite. The filled andalusite and the natural andalusite are not different in element types, elements contained in the filled organic glue are mainly C, H, O, the natural andalusite and the filled andalusite cannot be distinguished by utilizing an X-ray fluorescence spectrometer, the energy dispersion type X-ray fluorescence spectrometer tests and shows that main constituent elements of the andalusite are Si and Al, the pink andalusite contains Rb and Cs, the blue andalusite contains Fe, the elements of the filling cannot be detected by depending on element tests, and the existence of the filling cannot be judged;
the laser Raman spectrometer has an unobvious effect on distinguishing the natural andalusite from the filled andalusite, has a small difference in laser Raman spectrum between the natural andalusite and the filled andalusite, and can display a Raman peak different from the natural andalusite only when the laser Raman spectrometer detects a filler in a surface crack;
fourier transform infrared spectrum, the Fourier transform infrared spectrum of the natural andalusite is 1200-400cm-1The fingerprint area is mainly the structural vibration of Si-O-Si ring and Be-O, Al-O; at 4000-2000 cm-1The functional group region is mainly CO2Generated 2350-2390 cm-1Absorption platform of (1), 3033cm by NaH-1、3112cm-1、3166cm-1Characteristic absorptionPeak and Fe3+Formation of [ Fe ] from ions and water molecules in the channel2(OH)4]2+3234cm generated by multiple polymeric ions-1And (4) absorbing. The packed andalusite has vibration absorption at 2870cm except for the groups of the andalusite-1、2930cm-1、2965cm-1ubiquitous-CH3—、—CH2-absorption; at 3035cm-1、3057cm-1There is absorption by the benzene ring. The Fourier transform infrared spectrum can effectively distinguish natural andalusite from filled andalusite;
the analysis of the three-dimensional fluorescence spectrogram shows that the fluorescence of the natural andalusite is very weak, the characteristic fluorescence center is absent, and the relative intensity is within 500; the fluorescence centers of the packed andalusite are mainly single fluorescence centers of about 400nm and double fluorescence centers of 440nm and 465nm, and the excitation light sources are 340-360 nm and 380-400 nm respectively. The relative intensity of the fluorescent centers of packed andalusite is significantly higher than that of natural andalusite due to the aromatic compounds in the organic glue added during the packing process. Fluorescence spectrum analysis is an effective and rapid nondestructive testing means for distinguishing natural and filling-processed andalusite.
Finally, it should be noted that: in the description of the present invention, it should be noted that the terms "vertical", "upper", "lower", "horizontal", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The method for nondestructively identifying the filling treatment of the andalusite is characterized by comprising the following steps of:
the method comprises the following steps: selecting a andalusite sample;
step two: measuring by adopting an FP-8500 fluorescence spectrometer of JASCO;
step three: and (4) processing data, and comparing the fluorescence spectrum to accurately identify the andalusite.
2. The method for filling and processing the andalusite with nondestructive identification according to claim 1, wherein in the first step, the andalusite sample to be tested is selected without sample preparation.
3. The method for filling and processing the andalusite with nondestructive identification according to claim 1, wherein in the second step, the fluorescence spectrometer test mode is Emission, the sensitivity is Manual, wherein the PMT voltage of the sample BT-7 is 600V, the rest of the samples are 700V, the wavelength range of the excitation light source is 305 to 550nm, and the slit width is 5 nm; the emission wavelength range is 325-650 nm, the slit width is 2.5nm, the data interval is 1nm, and the scanning speed is 2000 nm/min.
4. The method for nondestructive identification, filling and processing of andalusite as claimed in claim 1, wherein in the third step, data processing is performed, the relative intensity of the fluorescence center of the filled andalusite is significantly stronger than that of the natural andalusite, the andalusite can be accurately identified by comparing the relative intensity of the three-dimensional fluorescence spectrum, the fluorescence which cannot be seen through the uv fluorescent lamp can be quantified by the high sensitivity of the fluorescence spectrometer, and the fluorescence intensity distribution of the gem within the whole excitation band can be completely shown by the irradiation of its continuous excitation light source.
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Cited By (1)
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| CN110779943A (en) * | 2019-10-23 | 2020-02-11 | 长春黄金研究院有限公司 | Identification method for dyeing natural turquoise |
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Application publication date: 20210910 |