CN107064043A - A kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder - Google Patents
A kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder Download PDFInfo
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- CN107064043A CN107064043A CN201710257519.1A CN201710257519A CN107064043A CN 107064043 A CN107064043 A CN 107064043A CN 201710257519 A CN201710257519 A CN 201710257519A CN 107064043 A CN107064043 A CN 107064043A
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- 239000000843 powder Substances 0.000 title claims abstract description 289
- 238000002156 mixing Methods 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 37
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 155
- 241000276489 Merlangius merlangus Species 0.000 claims abstract description 58
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 49
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 45
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000001354 calcination Methods 0.000 claims abstract description 30
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 50
- 238000010521 absorption reaction Methods 0.000 claims description 47
- 238000000227 grinding Methods 0.000 claims description 45
- 238000001514 detection method Methods 0.000 claims description 29
- 239000007787 solid Substances 0.000 claims description 26
- 229910018557 Si O Inorganic materials 0.000 claims description 24
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 24
- 239000002019 doping agent Substances 0.000 claims description 18
- 238000004566 IR spectroscopy Methods 0.000 claims description 11
- 238000001228 spectrum Methods 0.000 claims description 9
- 230000003595 spectral effect Effects 0.000 claims description 8
- 238000005242 forging Methods 0.000 claims 1
- 238000004451 qualitative analysis Methods 0.000 abstract description 7
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical group [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000391 magnesium silicate Substances 0.000 abstract description 5
- 229910052919 magnesium silicate Inorganic materials 0.000 abstract description 5
- 235000019792 magnesium silicate Nutrition 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000002790 cross-validation Methods 0.000 description 14
- 238000012937 correction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000007689 inspection Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012850 discrimination method Methods 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 235000012222 talc Nutrition 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 206010010904 Convulsion Diseases 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000004971 IR microspectroscopy Methods 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- -1 agricultural Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 238000001320 near-infrared absorption spectroscopy Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
The invention provides a kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder, using FFIR, qualitative and quantitative analysis is carried out to the oyster shell whiting of doubtful doping, Paris white, talcum powder in pearl powder to be measured.The general principle that the present invention is based on is：Calcium carbonate in pearl powder is aragonitic, calcium carbonate in Paris white is calcite type, oyster shell whiting is after specified temp calcining, and the calcium carbonate of aragonitic also will all be converted to the calcium carbonate of calcite type, and the calcium carbonate in pearl powder after calcining is remained in that as aragonitic；In addition, the main component of talcum powder is magnesium silicate, the Si O stretching vibration absworption peaks of wherein magnesium silicate also are located at middle infrared, and have significant difference with the characteristic peak of pearl powder.The middle infrared spectrum authentication method provided by the present invention for mixing pseudo- pearl powder has the advantages that sample preparation is rapid, analysis operation is simple, convenient and swift, error is small, expense is low, and therefore, it has superior scientific research value and market value.
Description
Technical field
The present invention relates to a kind of authentication method for mixing pseudo- pearl powder, more particularly to a kind of middle infrared spectrum for mixing pseudo- pearl powder
Authentication method.
Background technology
Pearl is medicinal in existing more than the 2000 years history of China,《Chinese Pharmacopoeia》And《Dictionary of medicinal plant》Indicate：Pearl
The effects such as with arresting convulsion of calming the nerves, shade removing, solution taking poison and growing muscle due, modern study also shows that pearl powder is improving body immunity, prolonged
All there is unique effect in terms of slow aging, freckle removing and whitening, supplement calcium.Pearl powder is used as a kind of Chinese medicine, its economic valency
Value is growing, but some illegal retailers are in order to obtain bigger interests, the oyster shell whiting that adulterated in pearl powder, Paris white,
Talcum powder etc. improves pearl powder whiteness, fineness, and reduces production cost, and this causes a large amount of fake and forged pearl powders to flow into cities
, pearl powder market order has seriously been confused, the physical and mental health of consumer is threatened.
In the prior art, people have carried out numerous studies, generally use the methods such as XRD, SEM, FTIR to differentiate pearl powder
And oyster shell whiting, however, these methods in terms of sample crystal formation, method for making sample, example weight, detection time to having strict limit
System.For example, Chinese patent CN101620176B discloses the discrimination method of a kind of pearl powder and oyster shell whiting, it is by pearl powder and shellfish
Shell powder is mixed and made into transparent sheet with KBr respectively after being calcined, and then determines infrared absorption spectroscopy and carries out Qualitative Identification.
And for example, Chinese patent CN103411895B discloses the near infrared spectrum identification method that a kind of pearl powder mixes puppet, this method application
The method for qualitative analysis of Fourier transformation near infrared reflectance spectroscopy combination similarity mode analysis, establishes doping
The similarity mode for mixing pseudo- pearl powder of general impurity differentiates model；Also, apply Fourier transformation near-infrared diffusing reflection spectrum
Analytical technology combination PLS quantitative analysis methods, establish pearl powder mass fraction in the pearl powder for doping oyster shell whiting and determine
Amount differentiates model, and realizes that pearl powder mixes quick effective discriminating of puppet with two models coupling applications.In addition, Chinese patent
CN103344573B discloses the infrared microscopy reflectance spectrum discrimination method of a kind of pearl powder and oyster shell whiting, and the discrimination method first will
Pearl powder and oyster shell whiting are calcined, then the pearl powder of preparation and oyster shell whiting sample are passed through into Fourier trasfonn infrared microscope spectrum
Instrument carries out Infrared Reflective Spectra detection, so that carrying out qualitative analysis according to the change of chromatogram characteristic peak identifies pearl powder and oyster shell whiting
Sample.Found by analysis, although, above method respectively has feature, still, and above method and other existing achievements in research are not
Report or be related to the qualitative and quantitative analysis model of pearl powder doping oyster shell whiting, Paris white and talcum powder.
In addition, between the seventies in last century till now more than 40 years, the development of FFIR (FTIR) technology
Very fast, its function constantly expands, and performance is constantly improved, nowadays, and infrared spectrum technology has obtained more and more extensive
Using.At present, FFIR is in the disciplinary studies such as material, food, biology, medicine, agricultural, mineral, environment
Have and widely use.It is well known that infra-red sepectrometry has, sample preparation is simple, detection is rapid, precision and high resolution, be applicable it is wide
General the features such as.Applications of the FTIR (including near-infrared, in infrared, far infrared) in terms of mineral qualitative and quantitative analysis, increasingly
Cause the attention of people.Wherein, DR-FTIR is a kind of analysis method for relying on infrared spectrum, can be to powdered solid sample
Group and molecular structure carry out qualitative and quantitative analysis；Also, the measurement of diffusing reflection infrared spectrum (DR-FTIR) needs to be equipped with
Diffusing reflection annex.
Because the main component of most common dopant oyster shell whiting in pearl powder is also calcium carbonate, calcium carbonate is inorganic as one kind
Oxysalt, it may have specific infrared absorption spectroscopy, CO therein3 2-The characteristic absorption peak of ion is located at middle infrared spectral region,
Therefore, how using DR-FTIR and in 4000cm-1~400cm-1In spectral region to it is doubtful mix pseudo- pearl powder carry out it is qualitative,
Quantitative measurement, while guarantee to identify Paris white, talcum powder, oyster shell whiting, the scientific research personnel for becoming association area grinds
Study carefully one of focus.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present inventor intends devising a kind of utilize in diffusing reflection
Infrared Fourier Transform Infrared Spectrum Technology carries out qualitative, Quantitative measurement method to doubtful pseudo- pearl powder of mixing；This hair
The general principle of bright provided authentication method is：The main component of pearl powder, oyster shell whiting and Paris white is calcium carbonate, carbon
Sour calcium is as a kind of inorganic oxysalt, with specific infrared absorption spectroscopy, wherein CO3 2-Absworption peak be located at mid-infrared light
Area is composed, the calcium carbonate of different crystal forms, its infrared absorption peak has differences, the calcium carbonate in pearl powder is aragonitic, Paris white
In calcium carbonate be calcite type, oyster shell whiting specified temp calcining after, the calcium carbonate of aragonitic is also by all side's of being converted to solutions
The calcium carbonate of stone-type, the calcium carbonate in pearl powder after calcining is remained in that as aragonitic；In addition, the main component of talcum powder is
The Si-O stretching vibration absworption peaks of magnesium silicate, wherein magnesium silicate also are located at middle infrared, and have substantially with the characteristic peak of pearl powder
Difference；Then, using the calcium carbonate of calcite type, the calcium carbonate of aragonitic, the Si-O of magnesium silicate characteristic absorption peak difference,
It can effectively distinguish pearl powder, oyster shell whiting, Paris white, talcum powder, also, by multiple infrared spectrums for mixing pseudo- pearl powder sample
Figure and specifically constituent content input TQ Analyst softwares mix the Quantitative Analysis Model of pseudo- pearl powder to set up, and are tested by intersecting
Card is verified to model, and calculates coefficient correlation and cross validation mean square deviation, for assessment models performance.
Therefore, based on above general principle, the invention provides a kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder,
It comprises the following steps：
S1：Using be equipped with diffusing reflection annex determination of infrared spectroscopy respectively containing pure Paris white, pure talcum powder,
The infrared detection KBr solid samples of pure oyster shell whiting after calcining, gather the infrared spectrogram of standard sample respectively, and obtain
：
The characteristic absorption peak of pure Paris white calcite type calcium carbonate corresponding with the pure oyster shell whiting after calcining；
The corresponding Si-O characteristic absorption peaks of pure talcum powder；
S2：Pearl powder to be measured is dried, calcined, sample preparation obtains the infrared detection KBr solid-likes containing pearl powder to be measured
Product；
S3：Use the obtained infrared inspection for containing pearl powder to be measured in the determination of infrared spectroscopy S2 of outfit diffusing reflection annex
KBr solid samples are surveyed, and gather the corresponding infrared spectrogram of pearl powder to be measured；
S4：Judge whether the feature containing the calcite type calcium carbonate is inhaled in the corresponding infrared spectrogram of pearl powder to be measured
Receive peak or/and the Si-O characteristic absorption peaks：
(1) if not containing the characteristic absorption peak and the Si-O characteristic absorption peaks of the calcite type calcium carbonate, then
Confirm that the pearl powder to be measured does not adulterate Paris white, talcum powder, oyster shell whiting；
(2) if the characteristic absorption peak containing the calcite type calcium carbonate and the Si-O characteristic absorption peaks, then really
Recognize the pearl powder to be measured and be doped with Paris white, talcum powder, oyster shell whiting；
(3) if comprising only the characteristic absorption peak of the calcite type calcium carbonate, then confirm that the pearl powder to be measured is mixed
Miscellaneous Paris white or/and oyster shell whiting, and undoped with talcum powder；
(4) if comprising only the Si-O characteristic absorption peaks, then confirm that the pearl powder to be measured is doped with talcum powder, and
Undoped with Paris white, oyster shell whiting.
What deserves to be explained is, TQ Analyst are a kind of general spectral analysis softwares, and it is infrared in being, near red
Outside, the application of far infrared and Raman spectrum analysis provides various qualitative and quantitative analysis instruments.
Preferably, the middle infrared spectrum authentication method of pseudo- pearl powder is mixed above-mentioned, the spy of the calcite type calcium carbonate
Levying absworption peak is：877cm-1~878cm-1；
The Si-O characteristic absorption peaks are：1018cm-1~1019cm-1。
Preferably, the middle infrared spectrum authentication method of pseudo- pearl powder is mixed above-mentioned, the condition of the calcining includes：In earthenware
In crucible, in calcining 10~30 minutes at 370 DEG C~420 DEG C.
Preferably, the middle infrared spectrum authentication method of pseudo- pearl powder is mixed above-mentioned, the sample preparation comprises the following steps：
Weigh in the pearl powder to be measured after calcining, the lid for pouring into mixed grinding bottle；KBr separately is weighed, mixing is poured into and grinds
Grind the bottom of bottle；Merge pearl powder to be measured and KBr after calcining in the mixed grinding bottle, then in mixing and grinding machine
Upper vibrations 1~2 minute, obtain sample mixture；Then, sample mixture is loaded into specimen cup, and scraped with slide to
Powder surface is flat, produces the infrared detection KBr solid samples for containing pearl powder to be measured.
Preferably, the middle infrared spectrum authentication method of pseudo- pearl powder is mixed above-mentioned, the infrared light of the collection standard sample
The condition of spectrogram and the corresponding infrared spectrogram of collection pearl powder to be measured is：Resolution ratio 4cm-1, scanning times 32 times adopt
The infrared spectrogram of collection is changed by Kubelka-Munk, spectral region 400cm-1~4000cm-1。
Wherein, all infrared spectrograms obtained are changed by Kubelka-Munk, so that each characteristic peak is more
It is easy to identified.
Preferably, in the S1 and S3 of the above-mentioned middle infrared spectrum authentication method for mixing pseudo- pearl powder, in addition to collection spectrum
The step of infrared spectrogram of pure KBr powder is as background spectrum.
More than step described in each preferred embodiment be used to Qualitive test it is doubtful mix pseudo- pearl powder (pearl to be measured
Powder), confirm whether doubtful the mixing is doped with Paris white, talcum powder, oyster shell whiting in pseudo- pearl powder.Certainly, this is being confirmed
It is doubtful to mix pseudo- pearl powder really after mixing pseudo- pearl powder, further accurately to detect the carbon mixed in pseudo- pearl powder
The content of sour calcium powder/talcum powder/oyster shell whiting.
Therefore, it is further preferred that the above-mentioned middle infrared spectrum authentication method for mixing pseudo- pearl powder also includes what is quantitatively detected
Step：
First, pure pearl powder is separately taken, the infrared spectrogram of pure pearl powder is measured according to S2, S3, pure pearl powder correspondence is confirmed
Aragonite calcium carbonate characteristic absorption peak be 864cm-1~865cm-1；
Secondly, measure the pure pearl powder containing gradient concentration according to S2, S3 and/or a series of of dopant mix pseudo- pearl powder
The infrared spectrogram of sample；Wherein, the dopant is selected from any of Paris white, talcum powder, oyster shell whiting or a variety of；
Again, the pure pearl powder containing gradient concentration and/or a series of of dopant are mixed into the infrared of pseudo- pearl powder sample
Spectrogram importing TQ Analyst softwares mix the Quantitative Analysis Model of pseudo- pearl powder to set up；
Finally, Paris white/cunning in pearl powder to be measured is quantitatively detected according to the Quantitative Analysis Model for mixing pseudo- pearl powder
The content of stone flour/oyster shell whiting.
Be made explanation, it is above-mentioned quantitatively detect the step of in, using pure Paris white or/and pure talcum powder or/
Uniformly mixed by a certain percentage with pure pearl powder with pure oyster shell whiting and be doped with Paris white or/and talcum powder to simulate respectively
Or/and oyster shell whiting mixes pseudo- pearl powder, that is, obtain a series of of the pure pearl powder containing gradient concentration and/or dopant
Mix pseudo- pearl powder sample；Wherein, every part of quality for mixing pseudo- pearl powder sample generally uses 0.5g~1.0g.
It is further preferred that mixing the middle infrared spectrum authentication method of pseudo- pearl powder above-mentioned, the gradient concentration is：
It is described to mix pseudo- pearl powder sample and contain 0%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 100%
Pure pearl powder.
It is further preferred that mix the middle infrared spectrum authentication method of pseudo- pearl powder above-mentioned, it is described to mix pseudo- pearl powder
Quantitative Analysis Model using PLS PLS quantitative analyses algorithm set up.In addition, user can implement to intersect
Checking calculates coefficient correlation and cross validation mean square deviation to be verified to model, to assessment models performance.
In addition, what should be illustrated is：1. identified using the middle infrared spectrum provided by the present invention for mixing pseudo- pearl powder
When method implements Qualitative Identification, when operating personnel obtain a pearl powder sample to be measured, if whether unknown in advance wherein mix
Miscellaneous Paris white, talcum powder, oyster shell whiting (i.e. generally dopant species are unknown), then unify first to be measured by this part
Pearl powder sample is calcined, then sample preparation, detection；If previously known be wherein only possible to doped with Paris white or/and cunning
Stone flour, then, calcination operation step can be omitted, and will directly be detected after this part of pearl powder sample sample preparation to be measured；2. this hair is used
When bright the provided middle infrared spectrum authentication method for mixing pseudo- pearl powder implements Quantitative measurement, due to generally before Quantitative measurement
Qualitative Identification is completed, now operating personnel specify that the dopant species in pearl powder sample to be measured, then, when contained
When dopant does not include oyster shell whiting, calcination operation step can also be omitted, and directly by after this part of pearl powder sample sample preparation to be measured
Detection.
In a word, relative to prior art, technical scheme provided by the present invention mainly has following technical advantage：It is described to mix
The middle infrared spectrum authentication method of pseudo- pearl powder has that sample preparation is rapid, analysis operation is simple, convenient and swift, error is small, expense is low
Advantage；, can be to dopant species not when the middle infrared spectrum authentication method for mixing pseudo- pearl powder is applied to Qualitative Identification
The pearl powder to be measured known is planted dopant and made doped with which kind of or which fast and accurately to be judged, described to mix in pseudo- pearl powder
When infrared spectrum authentication method is applied to Quantitative measurement, the concrete content of dopant can be made and fast and accurately detected, especially
It is that the Quantitative Analysis Model for mixing pseudo- pearl powder set up can be used for a long time as master pattern, so as to avoid building repeatedly
The troublesome operation of vertical Quantitative Analysis Model.In summary, the middle infrared spectrum identification side provided by the present invention for mixing pseudo- pearl powder
Method has superior scientific research value and market value.
Brief description of the drawings
Fig. 1 is the mid-infrared light spectrogram of pure pearl powder；
Fig. 2 is the mid-infrared light spectrogram for mixing pseudo- pearl powder for being doped with Paris white；
Fig. 3 is the mid-infrared light spectrogram for mixing pseudo- pearl powder for being doped with talcum powder；
Fig. 4 is the mid-infrared light spectrogram for mixing pseudo- pearl powder for being doped with oyster shell whiting do not calcined；
Fig. 5 is the mid-infrared light spectrogram for mixing pseudo- pearl powder for being doped with oyster shell whiting after calcining；
Fig. 6 is the mid-infrared light spectrogram of the calibration set for the Quantitative Analysis Model for mixing pseudo- pearl powder；
Fig. 7 is correction and the proof diagram for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with oyster shell whiting；
Fig. 8 is the cross validation figure for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with oyster shell whiting；
Fig. 9 is correction and the proof diagram for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with Paris white；
Figure 10 is the cross validation figure for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with Paris white；
Figure 11 is correction and the proof diagram for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with talcum powder；
Figure 12 is the cross validation figure for the Quantitative Analysis Model for mixing pseudo- pearl powder for being doped with talcum powder.
Embodiment
With reference to embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiment party
Formula.
A kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder, comprises the following steps：
S1：Using be equipped with diffusing reflection annex determination of infrared spectroscopy respectively containing pure Paris white, pure talcum powder,
The infrared detection KBr solid samples of pure oyster shell whiting after calcining, gather the infrared spectrogram of standard sample respectively, and obtain
：
The characteristic absorption peak of pure Paris white calcite type calcium carbonate corresponding with the pure oyster shell whiting after calcining；
The corresponding Si-O characteristic absorption peaks of pure talcum powder；
S2：Pearl powder to be measured is dried, calcined, sample preparation obtains the infrared detection KBr solid-likes containing pearl powder to be measured
Product；
S3：Use the obtained infrared inspection for containing pearl powder to be measured in the determination of infrared spectroscopy S2 of outfit diffusing reflection annex
KBr solid samples are surveyed, and gather the corresponding infrared spectrogram of pearl powder to be measured；
S4：Judge whether the feature containing the calcite type calcium carbonate is inhaled in the corresponding infrared spectrogram of pearl powder to be measured
Receive peak or/and the Si-O characteristic absorption peaks：
(1) if not containing the characteristic absorption peak and the Si-O characteristic absorption peaks of the calcite type calcium carbonate, then
Confirm that the pearl powder to be measured does not adulterate Paris white, talcum powder, oyster shell whiting；
(2) if the characteristic absorption peak containing the calcite type calcium carbonate and the Si-O characteristic absorption peaks, then really
Recognize the pearl powder to be measured and be doped with Paris white, talcum powder, oyster shell whiting；
(3) if comprising only the characteristic absorption peak of the calcite type calcium carbonate, then confirm that the pearl powder to be measured is mixed
Miscellaneous Paris white or/and oyster shell whiting, and undoped with talcum powder；
(4) if comprising only the Si-O characteristic absorption peaks, then confirm that the pearl powder to be measured is doped with talcum powder, and
Undoped with Paris white, oyster shell whiting.
In a preferred embodiment, the characteristic absorption peak of the calcite type calcium carbonate is：877cm-1~878cm-1；
The Si-O characteristic absorption peaks are：1018cm-1~1019cm-1。
In a preferred embodiment, the condition of the calcining includes：In crucible, in calcining 10 at 370 DEG C~420 DEG C
~30 minutes.
In a preferred embodiment, the sample preparation comprises the following steps：
Weigh in the pearl powder to be measured after calcining, the lid for pouring into mixed grinding bottle；KBr separately is weighed, mixing is poured into and grinds
Grind the bottom of bottle；Merge pearl powder to be measured and KBr after calcining in the mixed grinding bottle, then in mixing and grinding machine
Upper vibrations 1~2 minute, obtain sample mixture；Then, sample mixture is loaded into specimen cup, and scraped with slide to
Powder surface is flat, produces the infrared detection KBr solid samples for containing pearl powder to be measured.
In a preferred embodiment, the infrared spectrogram of the collection standard sample is corresponding with collection pearl powder to be measured
The condition of infrared spectrogram be：Resolution ratio 4cm-1, scanning times 32 times, the infrared spectrogram of collection passes through Kubelka-
Munk is changed, spectral region 400cm-1~4000cm-1。
In a preferred embodiment, the infrared spectrogram for also including gathering specpure KBr powder in S1 and S3 is made
The step of for background spectrum.
In a further preferred embodiment, the described middle infrared spectrum authentication method for mixing pseudo- pearl powder also includes
The step of quantitatively detecting：
First, pure pearl powder is separately taken, the infrared spectrogram of pure pearl powder is measured according to S2, S3, pure pearl powder correspondence is confirmed
Aragonite calcium carbonate characteristic absorption peak be 864cm-1~865cm-1；
Secondly, measure the pure pearl powder containing gradient concentration according to S2, S3 and/or a series of of dopant mix pseudo- pearl powder
The infrared spectrogram of sample；Wherein, the dopant is selected from any of Paris white, talcum powder, oyster shell whiting or a variety of；
Again, the pure pearl powder containing gradient concentration and/or a series of of dopant are mixed into the infrared of pseudo- pearl powder sample
Spectrogram importing TQ Analyst softwares mix the Quantitative Analysis Model of pseudo- pearl powder to set up；
Finally, Paris white/cunning in pearl powder to be measured is quantitatively detected according to the Quantitative Analysis Model for mixing pseudo- pearl powder
The content of stone flour/oyster shell whiting.
In an embodiment still more preferably, the gradient concentration is：It is described to mix pseudo- pearl powder sample and contain
0%th, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 100% pure pearl powder.Wherein, with up to a hundred
It is mass percentage content to divide than content；Also, respectively have 0%, 10%, 20%, 30%, 40%, 50%, 60%,
70%th, 11 parts of the pure pearl powder of 80%, 90%, 100% theoretical content mix one calibration set of pseudo- pearl powder sample composition, separately
3 parts of the outer pure pearl powder using the actual content respectively with 45%, 65%, 85% are mixed pseudo- pearl powder sample composition one and tested
Card collection.
In an embodiment still more preferably, the Quantitative Analysis Model for mixing pseudo- pearl powder is using partially minimum
Two multiply what recurrence PLS quantitative analyses algorithm was set up.
Embodiment 1
Containing Paris white or/and talcum powder, (the i.e. known pearl powder to be measured is only possible containing being used as dopant using doubtful
Paris white or/and talcum powder, then eliminate calcination operation) pearl powder to be measured drying, weigh 0.5g pearl powders to be measured
In sample, the lid for pouring into mixed grinding bottle；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；In the mixed grinding
Merge pearl powder sample to be measured and KBr in bottle, then shaken 1 minute on mixing and grinding machine, obtain sample mixture；Then,
Sample mixture is loaded into specimen cup, and is scraped with slide flat to powder surface, that is, is obtained containing pearl powder to be measured
Infrared detection KBr solid samples；
The infrared detection KBr solids for containing pearl powder to be measured described in the determination of infrared spectroscopy of diffusing reflection annex using being equipped with
Sample, and gather the corresponding infrared spectrogram of pearl powder to be measured；
Judge in the corresponding infrared spectrogram of pearl powder to be measured whether the characteristic absorption peak containing calcite type calcium carbonate or/
With Si-O characteristic absorption peaks：
CO in the corresponding aragonite calcium carbonate of pearl powder3 2-Out-of-plane bending vibration absworption peak appears in 865cm-1(such as Fig. 1
It is shown), the CO in the corresponding calcite type calcium carbonate of Paris white3 2-Out-of-plane bending vibration absworption peak appears in 877cm-1, talcum
The corresponding Si-O stretching vibration absworption peaks of powder appear in 1019cm-1；If occurring in that 865cm simultaneously in the infrared spectrogram-1With
877cm-1Characteristic absorption peak (as shown in Figure 2), then illustrate to be doped with Paris white in the pearl powder to be measured；If the infrared spectrogram
In simultaneously occur in that 865cm-1And 1019cm-1Characteristic absorption peak (as shown in Figure 3), then illustrate to be doped with the pearl powder to be measured
Talcum powder.
Embodiment 2
Pearl powder to be measured is dried, in crucible, in being calcined 25 minutes at 400 DEG C, then, 0.5g pearl powders to be measured are weighed
In sample, the lid for pouring into mixed grinding bottle；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；In the mixed grinding
Merge pearl powder sample to be measured and KBr in bottle, then shaken 1 minute on mixing and grinding machine, obtain sample mixture；Then,
Sample mixture is loaded into specimen cup, and is scraped with slide flat to powder surface, that is, is obtained containing pearl powder to be measured
Infrared detection KBr solid samples；
The infrared detection KBr solids for containing pearl powder to be measured described in the determination of infrared spectroscopy of diffusing reflection annex using being equipped with
Sample, and gather the corresponding infrared spectrogram of pearl powder to be measured；
Judge in the corresponding infrared spectrogram of pearl powder to be measured whether the characteristic absorption peak containing calcite type calcium carbonate or/
With Si-O characteristic absorption peaks：
CO in the corresponding aragonite calcium carbonate of pearl powder3 2-Out-of-plane bending vibration absworption peak appears in 865cm-1(such as Fig. 1
It is shown), the CO in the corresponding calcite type calcium carbonate of Paris white3 2-Out-of-plane bending vibration absworption peak appears in 877cm-1, talcum
The corresponding Si-O stretching vibration absworption peaks of powder appear in 1019cm-1, after oyster shell whiting calcining, aragonite calcium carbonate therein all turns
It is changed into calcite type calcium carbonate, the oyster shell whiting after calcining also correspond to the CO in calcite type calcium carbonate3 2-Out-of-plane bending vibration is inhaled
Receive peak 877cm-1；If the main characteristic absorption peak of only one of which in the infrared spectrogram of the pearl powder sample to be measured before calcining
865cm-1865cm is occurred in that in the infrared spectrogram of pearl powder sample to be measured after (as shown in Figure 4), and calcining simultaneously-1With
877cm-1Characteristic absorption peak (as shown in Figure 5), then illustrate to be doped with oyster shell whiting in the pearl powder to be measured.
Embodiment 3
First, according to the Theoretical Mass degree 0% of pure pearl powder, 10%, 20%, 30%, 40%, 50%,
60%th, 70%, 80%, 90%, 100%, the oyster shell whiting for the respective quality degree that adulterates obtains a series of mixing pseudo- pearl powder
Sample, they constitute a calibration set (set of correcting sample)；
Then, pseudo- pearl powder sample mixed grinding in mortar is mixed by every part uniformly, to move into crucible, at 400 DEG C
Calcining 25 minutes, then, every part weighs 0.5g and mixes in pseudo- pearl powder sample, the lid for pouring into mixed grinding bottle；Separately weigh
KBr, pours into the bottom of mixed grinding bottle；Merge in the mixed grinding bottle and mix pseudo- pearl powder sample and KBr, then exist
Shaken 1 minute on mixing and grinding machine, obtain sample mixture；Then, sample mixture is loaded into specimen cup, and uses slide
Scrape flat to powder surface, that is, obtain containing the infrared detection KBr solid samples for mixing pseudo- pearl powder；
Determined respectively described in 11 parts containing the infrared inspection for mixing pseudo- pearl powder using the infrared spectrometer for being equipped with diffusing reflection annex
KBr solid samples are surveyed, and the corresponding infrared spectrogram of pseudo- pearl powder (as shown in Figure 6) is mixed in collection；Wherein, infrared spectrogram is gathered
Condition is：Resolution ratio 4cm-1, scanning times 32 times, the infrared spectrogram of collection is by Kubelka-Munk conversions, spectral region
400cm-1~4000cm-1。
Then, the pure pearl powder containing gradient concentration and/or a series of of oyster shell whiting are mixed into the infrared of pseudo- pearl powder sample
Spectrogram imports TQ Analyst softwares, and pseudo- pearl powder is mixed to be set up using PLS PLS quantitative analyses algorithm
Quantitative Analysis Model；
Finally, quantitatively detected according to the Quantitative Analysis Model for mixing pseudo- pearl powder and mix containing for oyster shell whiting in pseudo- pearl powder
Amount.
In addition, being verified using cross validation to Quantitative Analysis Model, calculate coefficient correlation and cross validation is square
Difference, for assessment models performance：The Quantitative Analysis Model correction mean square deviation RMSEC set up is 2.11, coefficient correlation
Corr.Coeff. it is 0.9978；It is 0.650 to predict mean square deviation RMSEP, and coefficient correlation Corr.Coeff. is 1.0000 (such as Fig. 7
It is shown)；Cross validation mean square deviation RMSECV is 2.87, and coefficient correlation Corr.Coeff. is 0.9960 (as shown in Figure 8).
Further, using 3 of the pure pearl powder respectively with 45%, 65%, 85% actual mass degree
Part is doped with the pseudo- pearl powder sample of mixing of oyster shell whiting, moves into crucible, and in being calcined 25 minutes at 400 DEG C, then, every part weighs
0.5g is mixed in pseudo- pearl powder sample, the lid for pouring into mixed grinding bottle；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；
Merge in the mixed grinding bottle and mix pseudo- pearl powder sample and KBr, then shaken 1 minute on mixing and grinding machine, obtain sample
Product mixture；Then, sample mixture is loaded into specimen cup, and is scraped with slide flat to powder surface, that is, obtained
Contain the infrared detection KBr solid samples for mixing pseudo- pearl powder；3 parts are determined respectively using the infrared spectrometer for being equipped with diffusing reflection annex
It is described containing the infrared detection KBr solid samples for mixing pseudo- pearl powder, and to mix pseudo- pearl powder corresponding red for collection under the same conditions
External spectrum figure；The Quantitative Analysis Model set up more than mixes pseudo- pearl powder sample to known actual mass degree
Infrared spectrogram quantitatively calculated, obtain this 3 parts mass percentage contents for mixing the pearl powder in pseudo- pearl powder sample
Calculated value is respectively 47.60%, 64.18%, 84.47%, it was demonstrated that the calculated value obtained according to the Quantitative Analysis Model set up
And actual value deviation is smaller (＜ 5%).
It is good predictive that data above shows that set up Quantitative Analysis Model has, available for being doped with oyster shell whiting
Mix the quantitative analysis of pseudo- pearl powder.
Embodiment 4
First, according to the Theoretical Mass degree 0% of pure pearl powder, 10%, 20%, 30%, 40%, 50%,
60%th, 70%, 80%, 90%, 100%, the Paris white for the respective quality degree that adulterates obtains a series of mixing pseudo- pearl
Powder sample, they constitute a calibration set (set of correcting sample)；
Then, every part is mixed that pseudo- pearl powder sample mixed grinding in mortar is uniform, every part weighs 0.6g and mixes pseudo- pearl powder
In sample, the lid for pouring into mixed grinding bottle；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；In the mixed grinding
Merge in bottle and mix pseudo- pearl powder sample and KBr, then shaken 1 minute on mixing and grinding machine, obtain sample mixture；Then,
Sample mixture is loaded into specimen cup, and is scraped with slide flat to powder surface, that is, is obtained containing mixing pseudo- pearl powder
Infrared detection KBr solid samples；
Determined respectively described in 11 parts containing the infrared inspection for mixing pseudo- pearl powder using the infrared spectrometer for being equipped with diffusing reflection annex
KBr solid samples are surveyed, and the corresponding infrared spectrogram of pseudo- pearl powder is mixed in collection；Wherein, infrared spectrogram acquisition condition is：Differentiate
Rate 4cm-1, scanning times 32 times, the infrared spectrogram of collection is by Kubelka-Munk conversions, spectral region 400cm-1~
4000cm-1。
Then, the pure pearl powder containing gradient concentration and/or a series of of Paris white are mixed into the red of pseudo- pearl powder sample
External spectrum figure imports TQ Analyst softwares, and pseudo- pearl powder is mixed to be set up using PLS PLS quantitative analyses algorithm
Quantitative Analysis Model；
Finally, quantitatively detected according to the Quantitative Analysis Model for mixing pseudo- pearl powder and mix containing for Paris white in pseudo- pearl powder
Amount.
In addition, being verified using cross validation to Quantitative Analysis Model, calculate coefficient correlation and cross validation is square
Difference, for assessment models performance：The Quantitative Analysis Model correction mean square deviation RMSEC set up is 1.59, coefficient correlation
Corr.Coeff. it is 0.9979；It is 0.380 (as shown in Figure 9) to predict mean square deviation RMSEP；Cross validation mean square deviation RMSECV is
2.16, coefficient correlation Corr.Coeff. are 0.9962 (as shown in Figure 10).
Further, using 3 of the pure pearl powder respectively with 45%, 65%, 85% actual mass degree
Part is doped with the pseudo- pearl powder sample of mixing of Paris white, and every part weighs 0.6g and mixes pseudo- pearl powder sample, pours into mixed grinding bottle
Lid in；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；Merge in the mixed grinding bottle and mix pseudo- pearl powder
Sample and KBr, then shake 1 minute on mixing and grinding machine, obtain sample mixture；Then, sample mixture is loaded into sample
In product cup, and scraped with slide flat to powder surface, that is, obtained containing the infrared detection KBr solid-likes for mixing pseudo- pearl powder
Product；Determine solid containing the infrared detection KBr for mixing pseudo- pearl powder described in 3 parts respectively using the infrared spectrometer for being equipped with diffusing reflection annex
Body sample, and the corresponding infrared spectrogram of pseudo- pearl powder is mixed in collection under the same conditions；The quantitative analysis set up more than
Model is quantitatively calculated the infrared spectrogram for mixing pseudo- pearl powder sample of known actual mass degree, obtain this 3
The calculated value that part mixes the mass percentage content of pearl powder in pseudo- pearl powder sample is respectively 46.95%, 63.89%,
85.20%, it was demonstrated that the calculated value and actual value deviation obtained according to the Quantitative Analysis Model set up is smaller (＜ 5%).
It is good predictive that data above shows that set up Quantitative Analysis Model has, available for being doped with Paris white
The quantitative analysis for mixing pseudo- pearl powder.
Embodiment 5
First, according to the Theoretical Mass degree 0% of pure pearl powder, 10%, 20%, 30%, 40%, 50%,
60%th, 70%, 80%, 90%, 100%, the talcum powder for the respective quality degree that adulterates obtains a series of mixing pseudo- pearl powder
Sample, they constitute a calibration set (set of correcting sample)；
Then, every part is mixed that pseudo- pearl powder sample mixed grinding in mortar is uniform, every part weighs 0.7g and mixes pseudo- pearl powder
In sample, the lid for pouring into mixed grinding bottle；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；In the mixed grinding
Merge in bottle and mix pseudo- pearl powder sample and KBr, then shaken 1 minute on mixing and grinding machine, obtain sample mixture；Then,
Sample mixture is loaded into specimen cup, and is scraped with slide flat to powder surface, that is, is obtained containing mixing pseudo- pearl powder
Infrared detection KBr solid samples；
Determined respectively described in 11 parts containing the infrared inspection for mixing pseudo- pearl powder using the infrared spectrometer for being equipped with diffusing reflection annex
KBr solid samples are surveyed, and the corresponding infrared spectrogram of pseudo- pearl powder is mixed in collection；Wherein, infrared spectrogram acquisition condition is：Differentiate
Rate 4cm-1, scanning times 32 times, the infrared spectrogram of collection is by Kubelka-Munk conversions, spectral region 400cm-1~
4000cm-1。
Then, the pure pearl powder containing gradient concentration and/or a series of of talcum powder are mixed into the infrared of pseudo- pearl powder sample
Spectrogram imports TQ Analyst softwares, and pseudo- pearl powder is mixed to be set up using PLS PLS quantitative analyses algorithm
Quantitative Analysis Model；
Finally, quantitatively detected according to the Quantitative Analysis Model for mixing pseudo- pearl powder and mix containing for talcum powder in pseudo- pearl powder
Amount.
In addition, being verified using cross validation to Quantitative Analysis Model, calculate coefficient correlation and cross validation is square
Difference, for assessment models performance：The Quantitative Analysis Model correction mean square deviation RMSEC set up is 1.45, coefficient correlation
Corr.Coeff. it is 0.9989；It is 0.00523 (as shown in figure 11) to predict mean square deviation RMSEP；Cross validation mean square deviation RMSECV
For 4.76, coefficient correlation Corr.Coeff. is 0.9899 (as shown in figure 12).
Further, using 3 of the pure pearl powder respectively with 45%, 65%, 85% actual mass degree
Part is doped with the pseudo- pearl powder sample of mixing of talcum powder, and every part weighs 0.7g and mixes pseudo- pearl powder sample, pours into mixed grinding bottle
In lid；KBr separately is weighed, the bottom of mixed grinding bottle is poured into；Merge in the mixed grinding bottle and mix pseudo- pearl powder sample
Product and KBr, then shake 1 minute on mixing and grinding machine, obtain sample mixture；Then, sample mixture is loaded into sample
In cup, and scraped with slide flat to powder surface, that is, obtained containing the infrared detection KBr solid samples for mixing pseudo- pearl powder；
Determined respectively described in 3 parts containing the infrared detection KBr solids for mixing pseudo- pearl powder using the infrared spectrometer for being equipped with diffusing reflection annex
Sample, and the corresponding infrared spectrogram of pseudo- pearl powder is mixed in collection under the same conditions；The quantitative analysis mould set up more than
Type is quantitatively calculated the infrared spectrogram for mixing pseudo- pearl powder sample of known actual mass degree, obtains this 3 parts
The calculated value for mixing the mass percentage content of the pearl powder in pseudo- pearl powder sample is respectively 44.28%, 64.48%,
85.95%, it was demonstrated that the calculated value and actual value deviation obtained according to the Quantitative Analysis Model set up is smaller (＜ 5%).
It is good predictive that data above shows that set up Quantitative Analysis Model has, available for being doped with talcum powder
Mix the quantitative analysis of pseudo- pearl powder.
The specific embodiment of the present invention is described in detail above, but it is intended only as example, and the present invention is not limited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
Substitute also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (9)
1. a kind of middle infrared spectrum authentication method for mixing pseudo- pearl powder, it is characterised in that comprise the following steps：
S1：Contain pure Paris white, pure talcum powder respectively, through forging using the determination of infrared spectroscopy for being equipped with diffusing reflection annex
The infrared detection KBr solid samples of pure oyster shell whiting after burning, gather the infrared spectrogram of standard sample respectively, and obtain：
The characteristic absorption peak of pure Paris white calcite type calcium carbonate corresponding with the pure oyster shell whiting after calcining；Pure
The corresponding Si-O characteristic absorption peaks of talcum powder；
S2：Pearl powder to be measured is dried, calcined, sample preparation obtains the infrared detection KBr solid samples containing pearl powder to be measured；
S3：Use the obtained infrared detection for containing pearl powder to be measured in the determination of infrared spectroscopy S2 of outfit diffusing reflection annex
KBr solid samples, and gather the corresponding infrared spectrogram of pearl powder to be measured；
S4：Judge in the corresponding infrared spectrogram of pearl powder to be measured whether to contain the characteristic absorption peak of the calcite type calcium carbonate
Or/and the Si-O characteristic absorption peaks：
(1) if not containing the characteristic absorption peak and the Si-O characteristic absorption peaks of the calcite type calcium carbonate, then confirm
The pearl powder to be measured does not adulterate Paris white, talcum powder, oyster shell whiting；
(2) if the characteristic absorption peak containing the calcite type calcium carbonate and the Si-O characteristic absorption peaks, then confirm institute
State pearl powder to be measured and be doped with Paris white, talcum powder, oyster shell whiting；
(3) if comprising only the characteristic absorption peak of the calcite type calcium carbonate, then confirm that the pearl powder to be measured is doped with
Paris white or/and oyster shell whiting, and undoped with talcum powder；
(4) if comprising only the Si-O characteristic absorption peaks, then confirm that the pearl powder to be measured is doped with talcum powder, and do not mix
Miscellaneous Paris white, oyster shell whiting.
2. the middle infrared spectrum authentication method according to claim 1 for mixing pseudo- pearl powder, it is characterised in that the calcite
The characteristic absorption peak of type calcium carbonate is：877cm-1~878cm-1；
The Si-O characteristic absorption peaks are：1018cm-1~1019cm-1。
3. the middle infrared spectrum authentication method according to claim 1 for mixing pseudo- pearl powder, it is characterised in that the calcining
Condition includes：In crucible, in calcining 10~30 minutes at 370 DEG C~420 DEG C.
4. the middle infrared spectrum authentication method according to claim 1 for mixing pseudo- pearl powder, it is characterised in that the sample preparation bag
Include following steps：
Weigh in the pearl powder to be measured after calcining, the lid for pouring into mixed grinding bottle；KBr separately is weighed, mixed grinding is poured into small
The bottom of bottle；Merge pearl powder to be measured and KBr after calcining in the mixed grinding bottle, then shaken on mixing and grinding machine
It is dynamic 1~2 minute, obtain sample mixture；Then, sample mixture is loaded into specimen cup, and scraped with slide to powder
Surface is flat, produces the infrared detection KBr solid samples for containing pearl powder to be measured.
5. the middle infrared spectrum authentication method according to claim 1 for mixing pseudo- pearl powder, it is characterised in that the collection mark
The condition of the infrared spectrogram of quasi- sample and the corresponding infrared spectrogram of collection pearl powder to be measured is：Resolution ratio 4cm-1, sweep
Retouch number of times 32 times, the infrared spectrogram of collection is changed by Kubelka-Munk, spectral region 400cm-1~4000cm-1。
6. the middle infrared spectrum authentication method according to claim 1 for mixing pseudo- pearl powder, it is characterised in that in S1 and S3
Also include the step of infrared spectrogram of the specpure KBr powder of collection is as background spectrum.
7. according to the middle infrared spectrum authentication method according to any one of claims 1 to 6 for mixing pseudo- pearl powder, its feature exists
In, in addition to the step of quantitative detection：
First, pure pearl powder is separately taken, the infrared spectrogram of pure pearl powder is measured according to S2, S3, the corresponding text of pure pearl powder is confirmed
The characteristic absorption peak of stone-type calcium carbonate is 864cm-1~865cm-1；
Secondly, measure the pure pearl powder containing gradient concentration according to S2, S3 and/or a series of of dopant mix pseudo- pearl powder sample
Infrared spectrogram；Wherein, the dopant is selected from any of Paris white, talcum powder, oyster shell whiting or a variety of；
Again, by the pure pearl powder containing gradient concentration and/or a series of infrared spectrums for mixing pseudo- pearl powder sample of dopant
Figure importing TQ Analyst softwares mix the Quantitative Analysis Model of pseudo- pearl powder to set up；
Finally, according to the Quantitative Analysis Model for mixing pseudo- pearl powder quantitatively detect Paris white/talcum powder in pearl powder to be measured/
The content of oyster shell whiting.
8. the middle infrared spectrum authentication method according to claim 7 for mixing pseudo- pearl powder, it is characterised in that the gradient is dense
Degree is：It is described mix pseudo- pearl powder sample contain 0%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%,
100% pure pearl powder.
9. the middle infrared spectrum authentication method according to claim 7 for mixing pseudo- pearl powder, it is characterised in that described to mix pseudo- treasure
The Quantitative Analysis Model of pearl powder is set up using PLS PLS quantitative analyses algorithm.
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