Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof

A quality inspection method, pearl powder technology, applied in measuring devices, material analysis using radiation diffraction, scientific instruments, etc., can solve the problem of large differences in position and peak area, limited analysis conclusions of mother-of-pearl powder, and reproducible test results gender issues

Inactive Publication Date: 2012-10-03
浙江华才检测技术有限公司
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Problems solved by technology

However, the mother-of-pearl powder used in this study has removed the cuticle, so there is no denaturation and decomposition of organic matter, only calcium carbonate decomposition. This method can only be used to identify high-quality mother-of-pearl powder, and it is difficult to identify those that have not removed the cuticle. Mother-of-pearl powder and nacre powder with prismatic layer and cuticle
The study shows that the structure and composition of pearl powder and nacre powder are very similar, and the analysis conclusions about mother-of-pearl powder (shell powder) are limited to high-quality mother-of-pearl powder
In addition, the amount of test samples used by thermogravimetric analysis is small, mostly a few milligrams to more than ten milligrams, so the requirements for the uniformity of the test samples are very high. When other similar substances are mixed in the pearl powder, the test results have poor reproducibility. And the positions and peak areas of the exothermic and endothermic peaks of pearl powders with different particle sizes are quite different.
[0009] The cost of mother-of-pearl powder is low, and it often flows into the market as pearl powder or mixed with pearl powder. There are even other powders with similar appearance (such as cassia powder, talcum powder, calcium carbonate powder, flour, etc.) mixed with pearl powder. These inferior mixed powders or counterfeit pearl powders seriously affect the health and safety of consumers and hinder the healthy development of the pearl industry.

Method used

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  • Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof
  • Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof
  • Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0108] Example 1 Detecting the Quality of Pearl Powder, Mother-of-Pearl Powder and Mixed Powder by XRD Diffraction Method

[0109] The samples to be tested in this embodiment are pearl powders of various listed brands or prepared from cultured pearls and their mother mussel shells produced in Zhuji, Zhejiang Province according to the preparation method described in the present invention.

[0110] In this embodiment, the sample to be tested is analyzed by XRD diffraction method, and the quality of pearl powder is detected through comparative research to determine the quality index for identifying pearl powder.

[0111] 1. XRD analysis method and test conditions

[0112] (1) Instrument: XRD powder diffractometer, θ / θ or θ / 2θ goniometer, goniometer resolution, no instrument (intrinsic) broadening at around 2θ28°, standard sample (SRM1976 or SRML a B 6 ) measured full width at half maximum (FHWM) <0.07°2θ.

[0113] (2) Test conditions

[0114] CaK arf Radiation, DS / SS: 1°R...

Embodiment 2

[0117] Example 2 Testing the quality of pearl powder, mother-of-pearl powder and mixed powder by thermal analysis

[0118] 1. Thermogravimetry and test conditions

[0119] a) Turn on the thermogravimetric analyzer (DSC / TGA) for 30 minutes and turn on the air;

[0120] b) Return to zero after the balance reading is stable, open the furnace to remove the sample, and use α-Al 2 o 3 Fill the crucible with 10-15 mg of the sample to be tested and put it back, and turn off the furnace;

[0121] c) After the balance reading is stable, raise the temperature from room temperature to 800°C at a rate of 10°C / min, measure the TG / DTA curve, save the data file, and process the test data with the instrument software. The results are shown in Table 1.

[0122] As seen from Table 1, through DSC / TGA analysis, the organic matter content in the pearl powder is 3.5-5.0wt.%, wherein, the organic matter content in the coarse pearl powder is 4.3-5.0wt.%; The organic matter content in the pearl f...

Embodiment 3

[0123] Example 3 Analysis of Thermal Phase Transition Properties of Samples to be Tested by XRD Diffraction Method

[0124] The analysis conditions for the thermal phase transition of the sample to be tested in the XRD diffraction analysis method are: in the air atmosphere, put the sample to be tested into the high-temperature accessory environmental sample stage of the diffractometer, raise it to 360°C at a rate of 100°C / min, and keep it warm for 5 -10 minutes, then lowered to room temperature at a rate of 100°C / min, and collected the diffraction data of the sample in the range of 15-70° 2θ. The results are shown in Table 1.

[0125] The quality detection result of table 1 pearl powder, mother-of-pearl powder, mixed powder

[0126]

[0127]

[0128] It can be seen from Table 1 that in an air atmosphere, the sample to be tested was heated to 360°C at a rate of 100°C / min, kept for 5-10 minutes, and then lowered to room temperature at a rate of 100°C / min, and analyzed b...

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Abstract

The invention relates to a quality detecting method of the pearl powder and an application thereof. The quality detecting method comprises any one or combination of the following methods: 1) analyzing a sample to be detected by adopting an X-ray diffraction (XRD) method, wherein the content of calcite phase in the pearl powder is less than or equal to 4.0 wt.%, the content of aragonite phase is greater than or equal to 96.0 wt.%; and / or, 2) analyzing the sample to be detected by adopting DSC / TGA (differential scanning calorimetry / thermo gravimetric analyzer), wherein the content of organic matters in the pearl powder is 3.5-5.0 wt.%; and / or, 3) after heating the sample to be detected to any one temperature ranged from 200 DEG C to 450 DEG C, preserving the temperature for 5-10 minutes; after reducing the temperature to room temperature, taking out the sample to be detected; detecting the content of calcite phase in the pearl powder by adopting the XRD diffraction method, wherein the content of the calcite in the pearl powder is less than or equal to 15.0 wt.%. The detecting method provided by the invention has the advantages of strong specificity and good stability and reproducibility; furthermore, the detecting method is quick and sensitive, simple and convenient, exact, effective and interference-free.

Description

technical field [0001] The invention relates to a method for detecting the quality of pearl powder by XRD and its application, so as to improve the stability, reproducibility, consistency and controllability of the quality detection of pearl powder, thereby ensuring its curative effect and safety. Background technique [0002] Pearls are precious decorations and valuable Chinese herbal medicines. They contain 91-94% active calcium, 18 kinds of amino acids, more than 30 kinds of trace elements and rich vitamin B components. It has more than 2,000 years of drug use history in my country. [0003] Pearls are divided into two categories: seawater pearls and freshwater pearls. my country is the main producer of pearls and pearl powder in the world, accounting for about 75% of the world's total output. At present, only 8-10% of high-grade pearls and 30% of craft-grade pearls in my country's freshwater pearls can be processed into jewelry and handicrafts. Most pearls are difficult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/20G01N5/00
Inventor 阮华君廖杰
Owner 浙江华才检测技术有限公司
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