The control method of the genuineness of precious stones

 

(57) Abstract:

Usage: the invention relates to a technique of spectral-luminescent analysis of substances and can be used on the customs and forensics for rapid and accurate control of movement of precious stones and their substitution by other stones, including a fake. The essence is that the method is based on irradiation with short pulse electron beams under control of precious stones, the registration of the spectrum of the resulting pulse cathodoluminescence and comparing the obtained spectrum with passport data of stone. Moreover, the exposure and recording of the spectrum are at least two times: the first time - to create a spectral-luminescent passport stone, the second and subsequent times under the direct control of the authenticity of the stone at his repeated appearances at the checkpoint. Check the spectrum of the luminescence is carried out in the wavelength ranges of not less than: (610-780) nm for rubies, spinel, alexandrite and emerald: (450-780) nm for sapphire, (350-680) nm - precious varieties of quartz, diamonds and pave rhinestone. The method is non-destructive, does not require pre-treatment of camcontrol (not more than a few minutes) and its validity. 2 Il.

The invention relates to a technique of spectral-luminescent analysis of substances and can be used on the customs and forensics for rapid and accurate control of movement of precious stones and their substitution by other stones, including a fake.

A known method of monitoring the authenticity of the precious stone that came from the checkpoint and appeared on it the second and subsequent times [1] including irradiation with ultraviolet and x-rays, and determining the color of the resulting luminescence. The disadvantage of this method is that it is not independent and reliable diagnostics of mineral species requires the involvement of other complementary techniques, which significantly increases the time for the control.

There is a method of analysis of minerals and rocks [2] includes their exposure to pulsed electron beams, registration luminescence spectrum and determination by him of the mineral composition of rocks or identification of the mineral. The main disadvantage of this method is that it does not provide specific methods and recommendations for control and the principle of authenticity control (not potentialenemy of the invention is a method for the identification of luminescent minerals [3] consists in the fact, that is, the sample is irradiated with UV laser with a density of 0.5 MW/cm2and more, emit luminescence in a specific region of the spectrum, measure its characteristics, including the intensity of the luminescence in 10-7and 10-6after excitation of luminescence, determine the difference between the measured intensities, compare them with similar values for the standard and identify the mineral. The disadvantages of this method is that: it is applicable only for "luminescent under UV laser irradiation of minerals limited; a known method is used to identify a specific mineral cassiterite, not a precious stone; the spread of way to other minerals is not obvious; in a way not revealed to the principles of "personification", i.e. control of the authenticity of the same specimen of a mineral when it appears again.

The technical object of the present invention is to improve expressnet and reliability of authentication controls or substitution of precious stones "personification" of stones.

This task is carried out by irradiation of their pulsed electron beams, registration SP is for sapphires. (350-680) nm for precious varieties of quartz, diamonds and pave rhinestone or in the range (350-780) nm for all these precious stones. Moreover, this operation is carried out at least twice: once to create the spectral-luminescent passport precious stone, when this information is recorded in digital, graphic, or other form and is accompanied by additional information, such as date of passport, name of the stone, owner name, etc., and all this information is stored. The second time the operation is performed by repeated passage of a stone through the checkpoint, and then compare the newly obtained spectral-luminescent information from the passport. When matching wavelength characteristic spectral bands and lines with an accuracy better than 1 nm and the shape of the spectrum (relative intensity of the individual spectral bands and lines) with an accuracy better than 5-10% for each spectral band gemstone believe the same, otherwise stated, the substitution of stone.

In Fig. 1 shows the luminescence spectra of a number of gemstones: 1

emerald; 2 spinel; 3 alexandrite; 4 sapphire; 5 ruby; 6 citrine; 7 - amethyst. In Fig. 2 presents the sample spectral-lumines is actively lumines cent. The parameters of electron beams are selected in accordance with the mineral form of exposed stone. For the selection of these parameters can be used, for example the work of [2] the luminescence referred to as pulse or pulse-periodic cathodoluminescence [4] a Characteristic feature of such luminescence is the fact that the range and shape for a particular precious stone is its constant characteristics [4] (Fig. 1). Moreover, for each type of precious stone individuality is manifested in the fine structure of spectral bands. Thus the reproducibility of the position of the local maxima of intensity at the wavelength close to absolute and depends only on the accuracy of calibration of spectral instruments, through which a recording is made of the spectrum in the preparation of the passport and re-test audit. These operations can be conducted on different instruments, the calibration of which is in the specified wavelength range is easily accomplished with an accuracy better than 1nm. Determination of the wavelengths of the maxima of the spectral bands (due to their relatively large width (Fig. 1) and the presence of noise photodetector apparatus) is also easily done with the same accuracy. Position W is contracted by an amount greater than 1 nm (Fig. 1). That is, this accuracy is sufficient for the control of the substitution.

The reproducibility of the shape of the spectrum is determined by the noise photoresistive equipment. This value plays an important role in monitoring the substitution of stone precious stone of the same kind, such as sapphire, sapphire, including synthetic, and to bind the wavelengths of the maxima with the above accuracy. The reproducibility of the shape of the spectrum than 10% allows for this binding, and 5% reproducibility allows you to control substitution of stones stones of the same species.

In the above wavelength ranges centered characteristic spectral lines and bands of pulse cathodoluminescence respective precious stones, sufficient for reliable control of their authenticity. The expansion of these ranges does not lead to a significant increase in the reliability of control, but increase the complexity and partly to increase control time. While the narrowing of the specified spectral ranges leads to loss of essential information and dramatically reduces the quality and reliability of the control.

Thus, the wavelengths of the characteristic spectral bands and lines and form SSA with repeated exposures characteristics and can be used to control authentication or substitution of stone other close to it in color or fake stones. I.e., spectral-luminescent passport precious stone is like a "fingerprint" in criminology. At this time of registration of the spectrum of luminescence, due to its high intensity, does not exceed a few seconds [4] when using the computer, and the comparison of spectral-luminescent information with passport using computers and even visually does not exceed a few minutes.

The need to create a spectral-luminescent passport gemstone, the type of Fig. 2, evident especially in the case when it is necessary to establish the authenticity (identity) stones subjected to secondary and subsequent controls. In the case where control is carried out to determine the type of precious stone, then we can use the generalized spectral-luminescent passports of the type of Fig. 1 for each type of precious stones. However, in this case, the comparison should only be performed by the matching wavelength spectral bands and lines of luminescence, as the spectrum shape of precious stones of one group can vary greatly.

The proposed method is easily amenable to automation, which helps to further increase its expr is non-destructive, does not require pre-treatment of the stone and its removal from the frame.

The proposed method was specifically implemented as follows. Shown on Fig. 1 precious stones was exposed to pulsed electron beams from table compact electron accelerator with the following parameters: electron energy of 180 Kev; the electron current density of 100 A/cm2; pulse width 310-9c; pulse repetition rate of 5 Hz. Light emission luminescence was imaged on the entrance slit of polychromator, to the output aperture which was docked multi-channel sensor type CCD with 512 elements connected to the computer.

Originally recorded the luminescence spectrum of each indicated in Fig. 1 stone, and has made the passport of the type specified in Fig. 2, and the passport was recorded on a floppy disk and stored in this form. Re-registration of the spectrum was carried out through the month, and a year later on the same experimental setup. The coincidence of spectral information from the passport was not worse than 0.2 nm spectral composition and not less than 5% in the form of the spectrum.

The control method of the genuineness of precious stones, including the irradiation of a sample, recording the ranks values for reference characterized in that the irradiation of the sample perform high-current pulse there is no electronic beams, and irradiation, registration and recording of the spectrum of luminescence of the sample is carried out at least twice: once to create the standard spectral-luminescent passport controlled stone, the second time when it reappears stone at the checkpoint, and compare again the spectrum recorded with passport data, and the coincidence of the wavelengths of spectral lines and bands with an accuracy better than 1 nm and the spectrum shape with accuracy not worse than 10% of the stone is considered the same, and otherwise ascertain the substitution, the registration of luminescence is carried out in the wavelength ranges not less 610-780 nm for rubies, spinel, alexandrite and emerald; 450-780 nm for sapphire; 350-680 nm to gem varieties of quartz, diamonds and pave rhinestone.

 

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