Effect of Sample Quality Control on X-ray Diffraction Measurement Results

doi:10.19894/j.issn.1000-0518.220349

Chinese Journal of Applied Chemistry ›› 2023, Vol. 40 ›› Issue (5): 720-729.DOI: 10.19894/j.issn.1000-0518.220349

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Effect of Sample Quality Control on X-ray Diffraction Measurement Results

Juan XIAO, Zhi-Feng SHI, Jia LIU, Bing LI, Xin-Rong XU()

Medical Devices Research & Testing Center，South China University of Technology，Guangzhou 510006，China

Received:2022-10-25 Accepted:2023-03-18 Published:2023-05-01 Online:2023-05-26
Contact: Xin-Rong XU
About author:xxrong@scut.edu.cn
Supported by:
the State Key Laboratory for Manufacturing Systems Engineering(sklms2020023);Guangdong Provincial Drug Administration Science and Technology Innovation Project(2021YDZ04)

Abstract

Abstract:

The effect of hydroxyapatite （HA） samples in different quality states on X-ray diffraction （XRD） results has been investigated systematically. The effects of sample state （block， layered and powder， etc.）， experimental method selection （powder polycrystalline diffraction and thin film grazing incidence diffraction， etc.） and detection environmental conditions （temperature， humidity and X-ray irradiation） on XRD detection are investigated. The results show that， compared with the block sample of HA， the intensity of the characteristic XRD peak of the powder sample after grinding and sieving treatment is significantly enhanced. For HA multi-layered growth samples， the phase analysis of each layer can be accurately achieved by combining grazing incidence and conventional powder diffraction. The particle size， amount， and filling method of the HA powder sample can also affect the XRD detection. The results show that the characteristic peak intensity of the HA powder sample with a particle size of 37 μm is about twice that of the sample with a particle size of 137 μm. In addition， the vacant sample preparation in the middle of a small amount of samples can cause the peak position of the characteristic peak to shift from 31.8 to 31.4（°）， and the peak intensity decreases from 11213.68 to 601.65. Moreover， appropriate storage and detection methods can prevent and avoid erroneous detection and result analysis for samples with poor stability to ambient temperature and humidity. Thus， ensuring high-quality XRD detection data and ensuring experimental data quality requires comprehensive quality control.

Key words: Quality control of samples, X-ray diffractometer, Hydroxyapatite, Test effectiveness

CLC Number:

O657

Juan XIAO, Zhi-Feng SHI, Jia LIU, Bing LI, Xin-Rong XU. Effect of Sample Quality Control on X-ray Diffraction Measurement Results[J]. Chinese Journal of Applied Chemistry, 2023, 40(5): 720-729.

Figures/Tables 9

Fig.1 The diffraction peaks of HA block samples before and after crushing

Fig. 2 Scanning electron microscopy of HA powders with different morphologies： short stripy （A）， granulation （B）， short rod-like （C）； HA powders with different morphologies： diffraction pattern （D）， the height of diffraction peaks （E）， the FWHM of diffraction peaks （F）

Fig. 3 XRD patterns of HA blocks with different rotation angles （A）； The height of peaks （B）； The FWHM of peaks （C）； XRD patterns of HA powder with different rotation angles after particle size refinement （D）

Fig.4 XRD patterns of HA block samples tested in different diffraction modes

Fig. 5 SEM image of ungrinding（A） and grinding and sieving （B） of HA particles； XRD patterns under different treatment methods （C）

Fig.6 Effect of surface roughness of enough samples on diffraction peaks

Fig.7 The influence of different depth of sample on diffraction peaks

Fig.8 Influence of loading position of HA sample on diffraction peaks

Fig.9 XRD patterns of HA powder placed at 23 ℃ and humidity of 30%， 50% and 80% for 24 h （A）； XRD patterns of CaCl2 at 23 ℃ and 50% humidity for 2 h（B）； XRD patterns of HA powder by X-ray irradiation for 0， 0.5 and 1 h

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Effect of Sample Quality Control on X-ray Diffraction Measurement Results

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