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Method for Determination of Hydroxyapatite Content in β-Tricalcium Phosphate by Full Spectrum Refining

A technology of hydroxyapatite and refinement in tricalcium phosphate, which is applied in the field of chemical detection, can solve the problems of low accuracy of measurement results and unsatisfactory measurement results, and achieve the effect of saving money and time costs

Active Publication Date: 2022-02-25
SHANGHAI JIAOTONG UNIV
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Problems solved by technology

This method has only one diffraction peak for each phase selected into the calculation, and the test will be affected by the preferred crystal orientation and grain size, so the accuracy of the measurement results is not high
Others, such as the reference intensity method (RIR), K value method, etc., are also essentially based on single-peak calculations, and the accuracy of the measurement results is not ideal

Method used

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  • Method for Determination of Hydroxyapatite Content in β-Tricalcium Phosphate by Full Spectrum Refining
  • Method for Determination of Hydroxyapatite Content in β-Tricalcium Phosphate by Full Spectrum Refining
  • Method for Determination of Hydroxyapatite Content in β-Tricalcium Phosphate by Full Spectrum Refining

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Experimental program
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Effect test

Embodiment 1

[0021] This embodiment specifically includes the following steps:

[0022] Step 1. After grinding the β-TCP / HA mixture with an agate bowl, pass through a 250-mesh sieve;

[0023] Step 2. Weigh 0.5g±0.01g of the HA / β-TCP mixture, fill it into the sample stage of the diffractometer, make the compactness of the sample powder appropriate and the surface smooth, and then put it into the diffractometer for θ / θ coupling Scanning, the sample will rotate at a speed of 50 rpm during scanning, the start angle of 2θ scan is 5°, the end angle is 90°, and the step size is 0.02°;

[0024] Step 3. After collecting the diffraction data, import the diffraction spectrum into the phase search / matching analysis software, and determine that the main component of the sample is β-TCP and indeed contains HA;

[0025] Step 4, further carry out full-spectrum fitting quantitative analysis, analyze β-TCP with monoclinic crystal system, R-3m space group crystal structure and HA with hexagonal crystal syst...

Embodiment 2

[0029] The 2# sample was measured and the first-order Chebychev polynomial spectrum fitting calculation of the full background was carried out using TOPAS software, and the obtained sample β-TCP content was 96.74%, as shown in image 3 shown.

Embodiment 3

[0031] The 3# sample is measured and the background 3-level Chebychev polynomial full-spectrum fitting calculation is carried out using TOPAS software, and the obtained sample β-TCP content is 94.85%, such as Figure 4 shown.

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Abstract

A method for the full-spectrum refinement determination of hydroxyapatite content in β-tricalcium phosphate, by performing X-ray diffraction measurement on a β-TCP sample mixed with HA to obtain a high-resolution diffraction spectrum, using β-TCP crystals and HA The atomic space structure of the crystal is used as a template to construct the unit cell parameters and the crystal structure model, and then use the structure model as a constraint condition to perform qualitative detection of impurities in β-TCP and HA in the full spectrum range for each diffraction peak in the high-resolution diffraction spectrum Quantitative detection of full spectrum fit. The present invention is based on the correct analysis of the phase composition of the sample and the construction of a reasonable crystal structure for the phase components, and then takes all the diffraction peaks on the diffraction spectrum as the object of consideration, and comprehensively investigates the diffraction pattern of each phase in the tested sample. Overall status, a high-precision quantitative method for data processing via the Rietvelt method.

Description

technical field [0001] The present invention relates to a technique in the field of chemical detection, in particular to a method for determining the content of hydroxyapatite in β-tricalcium phosphate through refinement of the Rietveld method of XRD spectrum. Background technique [0002] β-TCP containing an appropriate amount of HA is currently a commonly used bioceramic material, and the content of HA will have an important impact on the physical and chemical properties of the final product. However, the ion detection technology based on the solution is not conducive to the detection of HA in high-purity β-TCP, while the existing pharmaceutical industry standard YY0683-2008, with the strongest diffraction peaks of β-TCP and HA (positions at 2θ= 31.0° and 31.8°) as the calculation basis, prefabricated standard samples with known content, developed a calibration curve by linear regression, and used the calibration curve to determine the HA content of unknown samples. Since...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/207
CPCG01N23/207
Inventor 饶群力
Owner SHANGHAI JIAOTONG UNIV
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