CN108132273A - A kind of method using x-ray fluorescence power spectrum identification porcelain pine - Google Patents

A kind of method using x-ray fluorescence power spectrum identification porcelain pine Download PDF

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CN108132273A
CN108132273A CN201810214022.6A CN201810214022A CN108132273A CN 108132273 A CN108132273 A CN 108132273A CN 201810214022 A CN201810214022 A CN 201810214022A CN 108132273 A CN108132273 A CN 108132273A
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porcelain
pine
ray fluorescence
sample
power spectrum
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曹姝旻
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

The present invention provides a kind of methods using x-ray fluorescence power spectrum identification porcelain pine, are related to identification method field.This method includes:It takes the genuine piece of porcelain pine that standard sample is made, using x-ray fluorescence spectroscopy analytical standard sample, obtains the classification and content of chemical element in porcelain pine;Multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, the chemical element data of porcelain pine is obtained, establishes the standard finger-print of porcelain pine;Turquoise sample preparation to be measured is taken to obtain sample to be tested, sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains the x-ray fluorescence power spectrum of sample to be tested, then be compared with standard finger-print.This method can carry out the chemical composition of porcelain pine qualitative and quantitative analysis by the wavelength and intensity of the characteristic X-ray spectral line for measuring chemical element, method high sensitivity, can effectively differentiate the true and false, the quality of porcelain pine.

Description

A kind of method using x-ray fluorescence power spectrum identification porcelain pine
Technical field
The present invention relates to identification method field, in particular to a kind of side using x-ray fluorescence power spectrum identification porcelain pine Method.
Background technology
Turquoise, also known as " turquoise " are gained the name because of its " the likeness in form pinecone, the nearly pine of color are green ".Color is to influence turquoise quality An important factor for.For turquoise because of the difference of contained element, color is also variant.In many turquoises, porcelain pine is turquoise In the prime quality, in bright-coloured sky blue, pure color, uniformly, gloss is strong, translucent to sub-translucent, and there are glass sense, matter in surface Ground is fine and close, fine and smooth, tough and tensile, no iron wire or other defect, and lumpiness is big.
However, with the progress of synthetic technology and preferred process technology, occur the composite of many turquoises in the market, this Kind composite and the difference of natural turquoise are less and less so that use traditional Identification Tools and means, it is difficult to which it is carried out It accurately distinguishes.Such as the conventional tools such as microscope, refractometer are mainly physical by the optical property and other that measure mineral Matter distinguishes turquoise, however these properties and parameter can only also make qualitatively qualification result, to optics or physical property class As stone cannot accomplish the differentiation that becomes more meticulous, this just make a part be located at edge zone stone be difficult to identify the true and false, and these Identification method is also difficult to identify the quality of turquoise quality, it is more difficult to which the quality of porcelain pine is identified.
Invention content
The purpose of the present invention is to provide a kind of methods using x-ray fluorescence power spectrum identification porcelain pine, and this method can Wavelength and intensity by the characteristic X-ray spectral line for measuring chemical element carry out the chemical composition of porcelain pine and turquoise qualitative And quantitative analysis, method high sensitivity, it can effectively differentiate the true and false and quality of porcelain pine.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme:
A kind of method using x-ray fluorescence power spectrum identification porcelain pine, including:
(1) it takes the genuine piece of porcelain pine that standard sample is made, using x-ray fluorescence spectroscopy analytical standard sample, obtains porcelain pine The classification and content of middle chemical element;
(2) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of porcelain pine, are established The standard finger-print of porcelain pine;
(3) turquoise sample preparation to be measured is taken to obtain sample to be tested, sample to be tested is analyzed using x-ray fluorescence spectroscopy, is treated The x-ray fluorescence power spectrum of sample, then be compared with standard finger-print.
Compared with prior art, beneficial effects of the present invention for example including:
This method using x-ray fluorescence power spectrum identification porcelain pine provided by the invention, by the spy for measuring chemical element The wavelength and intensity of X ray spectral line are levied, qualitative and quantitative analysis is carried out to the chemical composition of porcelain pine, so as to establish the standard of porcelain pine Finger-print.When detecting sample to be tested, it is only necessary to by its x-ray fluorescence power spectrum with and the standard finger-print of porcelain pine compare It is right, observe the wavelength and intensity of main characteristic X-ray spectral line, if this both in rational deviation range, as just Product.The high sensitivity of the identification method can effectively differentiate the true and false, the quality of porcelain pine.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
Present embodiment provides a kind of method using x-ray fluorescence power spectrum identification porcelain pine:
The principle of x-ray fluorescence spectroscopy is:The X-ray energy of irradiated atoms core and the energy of nuclear inner electron In the same order of magnitude, transition occurs after the radiation energy of the inner electron RESONANCE ABSORPTION ray of core, and in internal layer electron orbit On leave a hole, the hole of the outer-shell electron rebound lower state in upper state, by superfluous energy in the form of X ray It releases, generated X ray is the x-ray fluorescence spectral line for representing each element feature.Its energy is equal to atom inner-shell electron Energy level difference, i.e. the specific electronics interlayer transition energy of atom.Therefore, the wavelength of x-ray fluorescence is feature to different elements.
The identification method includes:
Step (1):It takes the genuine piece of porcelain pine that standard sample is made, the standard sample is analyzed using x-ray fluorescence spectroscopy, Obtain the classification and content of chemical element in the porcelain pine;
Further, it in the porcelain pine is obtained after the classification and content of chemical element, further includes and determines the porcelain pine again In characteristic chemical element.
Further, this feature chemical element is copper and phosphorus.
Further, the sample making course of porcelain pine or turquoise includes:By part porcelain pine or turquoise crush, take 3~5g (or Person is that 3.3~4.7g is either 3.6~4.4g or is 3.8~4.2g) turquoise powder, be pressed into a diameter of 45~ The print of 50mm (be either 46~49mm or be 47~78mm).Preferably, print surfacing, thickness for 0.5~ 1.5mm (be either 0.7~1.3mm be either 0.8~1.2mm or be 0.9~1.1mm).The sample of this size and thickness Piece, powder are uniformly dispersed, and translucency is good,, also can be by detector even if the fluorescence generated is very faint after being irradiated by X-rays It detects, during so as to avoid constituent content too low, can't detect or spectral line interference occur, help to improve the accuracy of analysis And sensitivity.
Step (2):Multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element of the porcelain pine Data establish the standard finger-print of the porcelain pine;
Further, after the standard finger-print of the porcelain pine is obtained, the spy for determining the porcelain pine again is further included The content range of chemical element is levied, wherein the content of the copper is 3.72~6.14% (or being 4.15~5.89%), it is described The content of phosphorus is 4.13~7.09% (or being 5.47~6.43%).The characterization in turquoise by determining particular color The content range of element is learned, quantitative analysis can be carried out to the element composition of this kind of turquoise, help to further improve identification Accuracy.
Further, the mass ratio of copper and the phosphorus is 1:1.2~1.8 or for 1.25~1.7.
Step (3):Turquoise sample preparation to be measured is taken to obtain sample to be tested, test sample is treated using described in the analysis of x-ray fluorescence spectroscopy Product obtain the x-ray fluorescence power spectrum of the sample to be tested, then are compared with the standard finger-print.
Further, the chemical element content for measuring the sample to be tested is further included, then judges copper and phosphorus in measurement result Whether the content of element is in the content range of the characteristic chemical element.
Further, x-ray fluorescence spectroscopy analysis is carried out using x-ray fluorescence energy disperse spectroscopy, x-ray fluorescence energy disperse spectroscopy Resolution ratio is less than 170eV, more preferably, resolution ratio be 150~165eV be either 153~162eV or be 157~ 160eV is 158~159eV.
The feature and performance of the present invention are described in further detail with reference to embodiments:
Embodiment 1
The present embodiment provides a kind of method using x-ray fluorescence power spectrum identification porcelain pine, this method uses x-ray fluorescence energy Spectrometer carries out, and the resolution ratio of the x-ray fluorescence energy disperse spectroscopy is 157~160eV.
This method includes:
(1) sample preparation:Part porcelain pine genuine piece or turquoise to be measured are crushed, 4g powder is taken to be pressed into the print of surfacing, A diameter of 45~47mm, thickness are 0.6~1.0mm, and standard sample and sample to be tested is made.
(2) standard sample of porcelain pine is taken, using x-ray fluorescence spectroscopy analytical standard sample, obtains chemistry member in porcelain pine The classification and content of element;
(3) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of porcelain pine, are established The standard finger-print of porcelain pine;
(4) sample to be tested is taken, sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains the x-ray fluorescence of sample to be tested Power spectrum, then be compared with standard finger-print.
The x-ray fluorescence power spectrum of the sample to be tested is more than 98% with standard finger-print similarity, you can concludes that this is to be measured Sample is the certified products of porcelain pine.
Embodiment 2
The present embodiment provides a kind of method using x-ray fluorescence power spectrum identification porcelain pine, this method uses x-ray fluorescence energy Spectrometer carries out, and the resolution ratio of the x-ray fluorescence energy disperse spectroscopy is 150~153eV.
This method includes:
(1) sample preparation:Part porcelain pine genuine piece or turquoise to be measured are crushed, 5g powder is taken to be pressed into the print of surfacing, A diameter of 47~49mm, thickness are 0.7~1.1mm, and standard sample and sample to be tested is made.
(2) standard sample of porcelain pine is taken, using x-ray fluorescence spectroscopy analytical standard sample, obtains chemistry member in porcelain pine The classification and content of element, then determine the characteristic chemical element in porcelain pine, as copper and phosphorus.
(3) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of porcelain pine, are established The standard finger-print of porcelain pine, and determine the content range of characteristic chemical element, i.e., the content of copper is 3.72~6.14%, phosphorus Content is 4.13~7.09%.
(4) sample to be tested is taken, sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains the x-ray fluorescence of sample to be tested Power spectrum and copper, the content of phosphorus are respectively 4.23%, 6.14%, then be compared with standard finger-print.
The x-ray fluorescence power spectrum of the sample to be tested is more than 96%, and wherein copper and phosphorus member with standard finger-print similarity The content of element is in above-mentioned content range, you can concludes the certified products that the sample to be tested is porcelain pine.
Embodiment 3
The present embodiment provides a kind of method using x-ray fluorescence power spectrum identification porcelain pine, this method uses x-ray fluorescence energy Spectrometer carries out, and the resolution ratio of the x-ray fluorescence energy disperse spectroscopy is 157~160eV.
This method includes:
(1) sample preparation:Part porcelain pine genuine piece or turquoise to be measured are crushed, 3g powder is taken to be pressed into the print of surfacing, A diameter of 48~50mm, thickness are 0.5~0.8mm, and standard sample and sample to be tested is made.
(2) standard sample of porcelain pine is taken, using x-ray fluorescence spectroscopy analytical standard sample, obtains chemistry member in porcelain pine The classification and content of element, then determine the characteristic chemical element in porcelain pine, as copper and phosphorus.
(3) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of porcelain pine, are established The standard finger-print of porcelain pine, and determine the content range of characteristic chemical element, i.e., the content of copper is 3.72~6.14%, phosphorus Content is 4.13~7.09%, and the mass ratio of copper and phosphorus is 1:1.2~1.8.
(4) sample to be tested is taken, sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains the x-ray fluorescence of sample to be tested Power spectrum and copper, the content of phosphorus are respectively 4.31%, 5.64%, then be compared with standard finger-print.
The x-ray fluorescence power spectrum of the sample to be tested is more than 96%, and wherein copper and phosphorus member with standard finger-print similarity The content of element is in above-mentioned content range, you can concludes the certified products that the sample to be tested is porcelain pine.
Embodiment 4
The present embodiment provides a kind of method using x-ray fluorescence power spectrum identification porcelain pine, this method uses x-ray fluorescence energy Spectrometer carries out, and the resolution ratio of the x-ray fluorescence energy disperse spectroscopy is 161~164eV.
This method includes:
(1) sample preparation:Part porcelain pine genuine piece or turquoise to be measured are crushed, 4g powder is taken to be pressed into the print of surfacing, A diameter of 48~50mm, thickness are 0.7~1.0mm, and standard sample and sample to be tested is made.
(2) standard sample of porcelain pine is taken, using x-ray fluorescence spectroscopy analytical standard sample, obtains chemistry member in porcelain pine The classification and content of element, then determine the characteristic chemical element in porcelain pine, as copper and phosphorus.
(3) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of porcelain pine, are established The standard finger-print of porcelain pine, and determine the content range of characteristic chemical element, i.e., the content of copper is 3.72~6.14%, phosphorus Content is 4.13~7.09%, and the mass ratio of copper and phosphorus is 1:1.2~1.8..
(4) sample to be tested is taken, sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains the x-ray fluorescence of sample to be tested Power spectrum and copper, the content of phosphorus are respectively 3.81% and 6.12%, then be compared with standard finger-print.
The x-ray fluorescence power spectrum of the sample to be tested is more than 96%, and wherein copper and phosphorus member with standard finger-print similarity The content of element is in above-mentioned content range, you can concludes the certified products that the sample to be tested is porcelain pine.
In conclusion this method using x-ray fluorescence power spectrum identification porcelain pine that the embodiment provides, passes through measure The wavelength and intensity of the characteristic X-ray spectral line of chemical element carry out qualitative and quantitative analysis, so as to build to the chemical composition of porcelain pine The standard finger-print of vertical porcelain pine.When detecting sample to be tested, it is only necessary to by its x-ray fluorescence power spectrum with and porcelain pine standard fingerprint Collection of illustrative plates is compared, and observes the wavelength and intensity of main characteristic X-ray spectral line, if both this is in rational deviation range It is interior, as certified products.The high sensitivity of the identification method can effectively differentiate the true and false, the quality of porcelain pine.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims Including belonging to all such changes and modifications in the scope of the invention.

Claims (9)

  1. A kind of 1. method using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that it includes:
    (1) it takes the genuine piece of porcelain pine that standard sample is made, the standard sample is analyzed using x-ray fluorescence spectroscopy, obtain described The classification and content of chemical element in porcelain pine;
    (2) multiple porcelain pine genuine pieces is taken to carry out x-ray fluorescence spectroscopy analysis, obtain the chemical element data of the porcelain pine, are established The standard finger-print of the porcelain pine;
    (3) turquoise sample preparation to be measured is taken to obtain sample to be tested, the sample to be tested is analyzed using x-ray fluorescence spectroscopy, obtains institute The x-ray fluorescence power spectrum of sample to be tested is stated, then is compared with the standard finger-print.
  2. 2. the method according to claim 1 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that step (1) In, in the porcelain pine is obtained after the classification and content of chemical element, further include the characteristic chemical member determined again in the porcelain pine Element.
  3. 3. the method according to claim 2 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that the feature Chemical element is copper and phosphorus.
  4. 4. the method according to claim 3 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that step (2) In, after the standard finger-print of the porcelain pine is obtained, further include and determine that the characteristic chemical element of the porcelain pine contains again Range is measured, wherein the content of the copper is 3.72~6.14%, the content of the phosphorus is 4.13~7.09%.
  5. 5. it is according to claim 4 using x-ray fluorescence power spectrum identification porcelain pine method, which is characterized in that the copper and The mass ratio of the phosphorus is 1:1.2~1.8.
  6. 6. the method according to claim 4 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that step (3) In, the chemical element content for measuring the sample to be tested is further included, then judge in measurement result the content of copper and P elements is whether In the content range of the characteristic chemical element.
  7. 7. the method according to claim 1 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that the porcelain pine Sample making course include:Part porcelain loose powder is broken, 3~5g porcelain loose powders end is taken to be pressed into the print of a diameter of 45~50mm.
  8. 8. the method according to claim 7 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that the print Surfacing, thickness are 0.5~1.5mm.
  9. 9. the method according to claim 1 using x-ray fluorescence power spectrum identification porcelain pine, which is characterized in that the X ray The analysis of fluorescence spectroscopy method is carried out using x-ray fluorescence energy disperse spectroscopy, and the resolution ratio of the x-ray fluorescence energy disperse spectroscopy is less than 170eV.
CN201810214022.6A 2018-03-15 2018-03-15 A kind of method using x-ray fluorescence power spectrum identification porcelain pine Pending CN108132273A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112946001A (en) * 2019-11-26 2021-06-11 中国科学院大连化学物理研究所 Component identification method for solid particle pollutants in solid-liquid laser cooling liquid
CN113189124A (en) * 2021-02-22 2021-07-30 中国地质大学(武汉) Method, system and medium for identifying turquoise by using silicate and porcelain treatment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112946001A (en) * 2019-11-26 2021-06-11 中国科学院大连化学物理研究所 Component identification method for solid particle pollutants in solid-liquid laser cooling liquid
CN113189124A (en) * 2021-02-22 2021-07-30 中国地质大学(武汉) Method, system and medium for identifying turquoise by using silicate and porcelain treatment

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Application publication date: 20180608