CN109444186A - A kind of pearl powder X-ray diffraction differential method - Google Patents
A kind of pearl powder X-ray diffraction differential method Download PDFInfo
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- CN109444186A CN109444186A CN201811587471.1A CN201811587471A CN109444186A CN 109444186 A CN109444186 A CN 109444186A CN 201811587471 A CN201811587471 A CN 201811587471A CN 109444186 A CN109444186 A CN 109444186A
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Abstract
The present invention provides a kind of pearl powder X-ray diffraction differential methods, comprising: the XRD diagram for acquiring pearl powder sample, shell powder sample respectively, as calibration set sample；Classify to calibration set sample, the optimal classification divisional plane of pearl powder and shell powder in discriminant analysis model is determined according to calibration set sample classification result；The XRD diagram of sample to be tested is acquired, object is carried out and mutually determines, to the sample to be tested for not containing aragonite phase, directly give the differentiation result of " unknown powder "；To the sample to be tested containing aragonite phase, differentiated with discriminant analysis model, obtains " pearl powder " or " shell powder " identification result.This method can distinguish the pearl powder containing aragonite phase, shell powder and the powder such as talcum powder, starch without aragonite phase, and the pearl powder containing aragonite phase and shell powder are classified in conjunction with chemometric model identification technology；It only can be realized with the XRD diagram of sample and pearl powder and a variety of fake products (shell powder, talcum powder, starch etc.) identified.
Description
Technical field
The invention belongs to the X-ray diffraction differential methods that pearl powder identifies field more particularly to a kind of pearl powder.
Background technique
Pearl powder is ground with the produced pearl of the shell-fishes such as hydriopsis cumingii, cristaria plicata, pteria martensii.Pearl
The medicinal history for having more than 2000 years in China of powder, the application field for being developed so far pearl powder have extended to health food, beauty
Hold the industries such as cosmetics, economic value multiplication.To seek exorbitant profit, illegal businessman using the appearances such as shell powder, talcum powder, starch with
The similar white powder of pearl powder pretends to be pearl powder to sell.Wherein the identification difficulty of shell powder and pearl powder is maximum, because of clam shell
It is similar to pearl chemical analysis, structure is similar, be processed into after powder and in appearance and be difficult to distinguish, conventional method is difficult to discriminate between.
It is existing research use the methods of scanning electron microscope, heat analysis, infrared/near infrared spectrum with identify pearl powder and
Parts or the partial informations such as the hot phase transformation difference of shell powder morphology, powder, characteristic group and key band difference
For distinguishing rule, these distinguishing rules are had some limitations.Application No. is 201110121080.2 patents to propose one
The method that kind identifies pearl powder and shell powder using X-ray diffraction combination heat analysis, this method need powder being heated to 400
DEG C, and a variety of instruments is needed to combine, it is cumbersome, take a long time.It is exactly known sample that these above-mentioned methods, which have an important prerequisite,
Product are pearl powder or shell powder, are only limitted to identify pearl powder and shell powder in these processes.And for totally unknown sample
Product depend merely on the above method and hardly result in ideal effect.
Pearl powder and shell powder are secreted by pearl secretory cell, ingredient be all by 5% or so organic matter and
95% or so calcium carbonate composition, wherein calcium carbonate is mainly combined by the aragonite crystals collection of sheet, plate.Due to pearl and its
The biological calcification environment of parent clam shell is different, and organic matter, inorganic element content and aragonite phase micro-structure have differences, penetrate in X
The nuance of peak type, position and intensity is then shown as in ray diffraction diagram spectrum, conventional method is difficult to seek from these nuances
Find the regular information that can distinguish the two.Chemical Measurement be one will be to chemical system by statistics or mathematical method
Measured value and system state between establish the subject contacted.This method is longer than applied mathematics, statistical method to greatest extent
Ground obtains ingredient, structure and other relevant informations in relation to material system.
Summary of the invention
The purpose of the present invention is to provide a kind of pearl powder X-ray diffraction differential method, this method can will contain aragonite phase
Pearl powder, shell powder distinguishes with the powder such as talcum powder, starch without aragonite phase, and combines chemometrics method will
Pearl powder and shell powder containing aragonite phase are classified；Only it can be realized with the XRD diagram of sample to pearl powder and a variety of personations
Product (shell powder, talcum powder, starch etc.) is identified.
The present invention achieves the above technical objects by the following technical means.
A kind of pearl powder X-ray diffraction differential method, comprising the following steps:
(1) XRD diagram for acquiring pearl powder sample, shell powder sample respectively, as calibration set sample；
(2) classify to calibration set sample, pearl in discriminant analysis model is determined according to calibration set sample classification result
The optimal classification divisional plane of powder and shell powder；If sample to be tested is located at divisional plane pearl powder side, discriminant analysis model provides " precious
Pearl powder " differentiates result；If sample to be tested is located at divisional plane shell powder side, discriminant analysis model provides " shell powder " and differentiates knot
Fruit；
(3) XRD diagram for acquiring sample to be tested carries out object and mutually determines, to the sample to be tested for not containing aragonite phase, directly gives
The differentiation result of " unknown powder "；To the sample to be tested containing aragonite phase, differentiated with the discriminant analysis model of step (2),
Obtain " pearl powder " or " shell powder " identification result.
In step (1), the pearl powder sample of acquisition, shell powder sample size are greater than 10.It is sufficiently ground with agate mortar
Grind away product simultaneously make sample by carrying out XRD diagram acquisition as sample after 300 meshes.
In step (1), the condition of XRD diagram is acquired are as follows: Cu K α 1, power 40Kv × 40mA, DS1 °, auto-changing air
Scatter slit, the θ mode of θ/2 scan, and 0.02 °/step, 0.2s/step, 20 °~90 ° of scanning range.
In step (2), the acquisition process of the calibration set sample classification result are as follows:
(2-1) carries out Pretreated spectra to the XRD diagram in calibration set sample；
(2-2) carries out Variable Selection to the XRD diagram after carrying out Pretreated spectra, obtains optimal variable, and the variable is to spread out
Firing angle；
(2-3) classifies the optimal variable that screening obtains with clustering method, obtains calibration set sample classification result.
In step (2-1), the Pretreated spectra is selected from multiplicative scatter correction, smooth, mean value centralization, standard normal
One of change of variable or derivative processing or at least two combination.
In step (2-2), the method for the Variable Selection be selected from correlation coefficient process, method of analysis of variance, method of gradual regression,
The null method of no information variable, the adaptive weight weight sampling method of competition, interval partial least square or genetic algorithm.
In step (2-3), the clustering method is selected from and is locally linear embedding into method, Principal Component Analysis, offset minimum binary
Method or artificial neural network method.
Preferably, the method for the Variable Selection is the adaptive weight weight sampling method of competition, based on the clustering method at
Divide analytic approach.The adaptive weight weight sampling method of competition is that one kind is based on Monte Carlo sampling and offset minimum binary (PLS) returns system
Several Variable Selection methods, this method select calibration set sample to establish corresponding PLS model by Monte Carlo sampling, and calculating is adopted
The absolute value weight of variable regression coefficient in sample, and the lesser variable of absolute value is removed by damped expoential method, then again based on surplus
Remaining variable repeats aforesaid operations, therefore the preferred variable successive optimization of this method selection, may finally select and be best able to body
The key variables of existing sample characteristics.Principal component analysis has the advantage of rapidly extracting principal component in more correlated variables of comforming, and is one
The important dimension reduction method of kind.
In step (3), the method that Discriminating materials are carried out to XRD diagram are as follows:
(3-1) calculates diffraction surfaces interplanar distance d value according to bragg's formula, and d value is arranged from big to small according to intensity；
(3-2) retrieval from last eight d value whether there is aragonite phase three strongest peak；If aragonite phase three strongest ones are not present in search result
Peak then illustrates that sample without aragonite phase, provides " unknown powder " and determines result；If search result there are aragonite phase three strongest peak,
Aragonite phase top eight peak is retrieved in all d values, and if it exists, illustrate sample phase containing aragonite.
In step (3), the sample to be tested includes pearl powder and appearance white powder similar with pearl powder, described outer
It sees white powder similar with pearl powder and is selected from shell powder, talcum powder or starch.
In the present invention, it can use verifying collection Sample discriminant analysis model accuracy, choosing verifying collection sample just
The discriminant analysis model of rate > 90% is sentenced as final Model checking analysis model.
Pearl powder X-ray diffraction differential method provided by the invention, X-ray diffraction is mutually determined with object and Chemical Measurement mould
Formula recognition methods combines, this method have the characteristics that it is easy, quick, reliable, be suitable for pearl powder relevant industries field carry out
It promotes and applies.
Detailed description of the invention
Fig. 1 is the XRD diagram of pearl powder provided in an embodiment of the present invention and shell powder；
Fig. 2 is 2 principal component scores scatter plots before pearl powder provided in an embodiment of the present invention and shell powder XRD diagram.
Specific embodiment
With specific embodiment, the present invention is further illustrated with reference to the accompanying drawing, and the description of this part is only exemplary
With it is explanatory, should not have any restriction effect to protection scope of the present invention.
Pearl powder X-ray diffraction differential method provided by the invention the following steps are included:
S1, the XRD diagram for acquiring pearl powder, shell powder, talcum powder, starch respectively.
Specifically, in the present embodiment, for the authenticity for ensuring pearl powder and shell powder, buying pearl respectively in market
16, sample, 16, clam shell sample.It is crushed respectively by pearl and with the clam shell of strong base solution removal cutin, grinds, crosses 300 mesh
Sieve, is made 16 pearl powder samples and 16 shell powder samples.Pearl powder sample number into spectrum is P1-P16, and wherein P1-P13 is pearl
Powder calibration set sample, P14-P16 is as sample to be tested；Shell powder sample number into spectrum is S1-S16, and wherein S1-S13 is shell powder school
Positive collection sample, S14-S16 is as sample to be tested.
Then P1-P13, S1-S13 sample XRD diagram, XRD instrument acquisition condition are as follows: Cu K α 1, function are acquired using XRD instrument
Rate 40Kv × 40mA, DS1 °, auto-changing air scattering slit, the θ mode of θ/2 scans, 0.02 °/step, 0.2s/step, scanning
20 °~90 ° of range.Fig. 1 is pearl powder and shell powder calibration set sample typical case's XRD diagram.
S2, classify to calibration set sample, pearl in discriminant analysis model is determined according to calibration set sample classification result
The optimal classification divisional plane of powder and shell powder；If sample to be tested is located at divisional plane pearl powder side, discriminant analysis model provides " precious
Pearl powder " differentiates result；If sample to be tested is located at divisional plane shell powder side, discriminant analysis model provides " shell powder " and differentiates knot
Fruit.
It is S201, smooth with Savitzky-Golay convolution to calibration set sample XRD diagram using matlab software self-compiling program
Method is smoothed to spectrum and second dervative processing.
S202, Variable Selection is carried out using competition adaptive weight weight sampling method to pretreated XRD diagram, screening obtains
Optimal variable in the angle of diffraction angle be 26.04,26.18,26.20,26.22,32.93,37.88,38.07,38.58,
41.32、43.06、45.80、48.30、48.50、52.43、53.01、77.23、77.32。
S203, the optimal variable that screening obtains is classified with principal component analysis dimension reduction method, Fig. 2 is pearl powder and freshwater mussel
2 principal component scores scatter plots before shell powder correcting sample XRD diagram, from figure 2 it can be seen that correcting sample pearl powder and shell powder
Significantly it is divided into two classes, and category attribution is all accurate.
S204, optimal classification divisional plane is determined according to calibration set sample classification result, as shown in phantom in Figure 2.
S3, the XRD diagram for acquiring sample to be tested, including pearl powder P14-P16, the shell powder S14-S16 in step S1；Also wrap
Talcum powder and starch are included, talcum powder and starch are purchased from market, and 16 talcum powder samples and 16 are made after crossing 300 meshes in grinding
A starch sample, talcum powder number are F1-F16, and starch sample number is A1-A16.
Object is carried out to the data of acquisition mutually to determine, to the sample to be tested for not containing aragonite phase, directly gives " unknown powder "
Differentiation result.To the sample to be tested containing aragonite phase, is differentiated with the discriminant analysis model of step S2, obtain " pearl powder "
Or " shell powder " identification result.
Specifically, in the present embodiment, the detailed process of identification are as follows:
S301, the diffraction that each sample (P14-P16, S14-S16, F1-F16, A1-A16) is calculated according to bragg's formula
Face interplanar distance d value, and d value is arranged from big to small according to intensity；
S302, retrieval whether there is aragonite phase three strongest peak (d=3.397,2.702,1.977) from last eight d value；If inspection
Aragonite phase three strongest peak is not present in hitch fruit, then illustrates that sample without aragonite phase, provides " unknown powder " and determines result.
In the present embodiment, aragonite phase three strongest ones are not present in the last eight d value of sample talcum powder F1-F16, starch A1-A16
Peak provides " unknown powder " and determines result.
If there are aragonite phase three strongest peaks for S303, S302 search result, aragonite phase top eight peak (d=is retrieved in all d values
3.397,2.702,1.977,3.274,2.373,2.481,2.108,1.743)；
If S304, S303 search result there are aragonite phase top eight peak, prove that sample main phase is aragonite phase, with step S2's
Discriminant analysis model is determined.
In the present embodiment, sample to be tested P14-P16, S14-S16, F1-F16, A1-A16 are adopted according to calibration set sample
Collection condition acquires sample to be tested XRD diagram, object phase determination step is carried out using the method for the present invention, for talcum powder F1-F16, starch
A1-A16, method directly give the differentiation result of " unknown powder "；For pearl powder P14-P16, shell powder S14-S16, in mould
In type decision process, pearl powder and shell powder verification sample principal component scores scatterplot are as shown in Figure 2, it can be found that P14-P16
It is identified as " pearl powder ", and S14-S16 is identified as " shell powder ", verification sample ownership is correct, model right judging rate
100%, which can be as the discriminant analysis model of final pearl powder X-ray diffraction discrimination method.
It can be seen from the figure that pearl powder X-ray diffraction discrimination method of the present invention can not be belonged to according to sample
Property, mutually determine that providing " unknown powder ", " shell powder " or " pearl powder " respectively with model decision process differentiates as a result, should by object
Method can be used for the pearl powder true and false and quickly identify, and this method is accurate, reliable.
Above embodiments are only that embodiments of the present invention are described, and are not defined to the scope of the invention,
Without departing from the spirit of the design of the present invention, those skilled in the art to make any aobvious of technical solution of the present invention and
The modification and improvement being clear to should belong in the protection scope that claims of the present invention determines.
Claims (9)
1. a kind of pearl powder X-ray diffraction differential method, which comprises the following steps:
(1) XRD diagram for acquiring pearl powder sample, shell powder sample respectively, as calibration set sample；
(2) classify to calibration set sample, according to calibration set sample classification result determine in discriminant analysis model pearl powder and
The optimal classification divisional plane of shell powder；If sample to be tested is located at divisional plane pearl powder side, discriminant analysis model provides " pearl
Powder " differentiates result；If sample to be tested is located at divisional plane shell powder side, discriminant analysis model provides " shell powder " and differentiates result；
(3) XRD diagram for acquiring sample to be tested carries out object and mutually determines, to the sample to be tested for not containing aragonite phase, directly gives " not
Know powder " differentiation result；To the sample to be tested containing aragonite phase, is differentiated with the discriminant analysis model of step (2), obtained
" pearl powder " or " shell powder " identification result.
2. pearl powder X-ray diffraction differential method according to claim 1, which is characterized in that in step (1), acquire XRD
The condition of figure are as follows: Cu K α 1, power 40Kv × 40mA, DS1 °, auto-changing air scattering slit, the θ mode of θ/2 scans,
0.02 °/step, 0.2s/step, 20 °~90 ° of scanning range.
3. pearl powder X-ray diffraction differential method according to claim 1, which is characterized in that in step (2), the school
The acquisition process of positive collection sample classification result are as follows:
(2-1) carries out Pretreated spectra to the XRD diagram in calibration set sample；
(2-2) carries out Variable Selection to the XRD diagram after carrying out Pretreated spectra, obtains optimal variable, and the variable is the angle of diffraction；
(2-3) classifies the optimal variable that screening obtains with clustering method, obtains calibration set sample classification result.
4. pearl powder X-ray diffraction differential method according to claim 3, which is characterized in that described in step (2-1)
Pretreated spectra is selected from one of multiplicative scatter correction, smooth, mean value centralization, standard normal variable transformation or derivative processing
Or at least two combination.
5. pearl powder X-ray diffraction differential method according to claim 3, which is characterized in that described in step (2-2)
The method of Variable Selection is selected from correlation coefficient process, method of analysis of variance, method of gradual regression, the null method without information variable, competition certainly
Adapt to weight weight sampling method, interval partial least square or genetic algorithm.
6. pearl powder X-ray diffraction differential method according to claim 3, which is characterized in that described in step (2-3)
Clustering method is selected from and is locally linear embedding into method, Principal Component Analysis, Partial Least Squares or artificial neural network method.
7. pearl powder X-ray diffraction differential method according to claim 5 or 6, which is characterized in that the side of the Variable Selection
Method is the adaptive weight weight sampling method of competition, and the clustering method is Principal Component Analysis.
8. pearl powder X-ray diffraction differential method according to claim 1, which is characterized in that described right in step (3)
The method of XRD diagram progress Discriminating materials are as follows:
(3-1) calculates diffraction surfaces interplanar distance d value according to bragg's formula, and d value is arranged from big to small according to intensity；
(3-2) retrieval from last eight d value whether there is aragonite phase three strongest peak；If aragonite phase three strongest peak is not present in search result,
Illustrate that sample without aragonite phase, provides " unknown powder " and determines result；If there are aragonite phase three strongest peaks for search result, all
Aragonite phase top eight peak is retrieved in d value, and if it exists, illustrate sample phase containing aragonite.
9. pearl powder X-ray diffraction differential method according to claim 1, which is characterized in that in step (3), it is described to
Sample includes pearl powder and appearance white powder similar with pearl powder, appearance white powder choosing similar with pearl powder
From shell powder, talcum powder or starch.
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| CN113390909A (en) * | 2021-06-11 | 2021-09-14 | 安徽理工大学 | Coal and gangue identification method based on X-ray diffraction technology |
| CN116559210A (en) * | 2023-03-21 | 2023-08-08 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
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| CN116559210A (en) * | 2023-03-21 | 2023-08-08 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
| CN116559210B (en) * | 2023-03-21 | 2024-04-30 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
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