样品质量控制对X射线衍射测量结果的影响  

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

作　　者：肖娟[1] 石志锋[1] 刘佳[1] 李冰[1] 徐昕荣[1] XIAO Juan;SHI Zhi-Feng;LIU Jia;LI Bing;XU Xin-Rong(Medical Devices Research&Testing Center,South China University of Technology,Guangzhou 510006,China)

机构地区：[1]华南理工大学医疗器械研究检验中心,广州510006

出　　处：《应用化学》2023年第5期720-729,共10页Chinese Journal of Applied Chemistry

基　　金：机械制造系统工程国家重点实验基金项目(No.sklms2020023);广东省药品监督管理局科技创新项目(No.2021YDZ04)资助。

摘　　要：以生物材料羟基磷灰石(HA)为样品模型,系统研究了HA样品在不同质量状态下对X射线衍射测试结果的作用。通过考察样品状态确认(块体、层状和粉末等)、实验方法选择(粉末多晶衍射和薄膜掠入射衍射等)以及环境条件控制(温度、湿度及X射线下辐照时间等)等因素,评价样品的质量控制对X射线衍射(XRD)检测数据准确性与真实性的影响。结果表明,与HA块状样品相比,经过研磨过筛处理后的粉末试样XRD特征峰强度显著增强,差异可增加至1倍以上。针对HA多层状生长样品,结合掠入射和常规粉末衍射可精准实现各层物相解析。HA粉末样品的粒径、样品量及对应的装填方式会影响XRD检测结果,粒径37μm的HA粉末样品的特征峰强是粒径137μm样品1倍左右;而少量样品的中部空置制样,可导致特征峰峰位由31.8(°)偏移至31.4(°),峰强从11213.68降到601.65。另外,对于稳定性不佳或对环境温湿度敏感的试样,采取合适的保存和检测方式,可有效预防和避免错误的检测与结果分析。因此,全面的质量控制对高质量的XRD检测数据获取和确保实验数据质量至关重要。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 37μm is about twice that of the sample with a particle size of 137μm.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.

关 键 词：质量控制 X射线衍射 羟基磷灰石 测试有效性 

分 类 号：O657[理学—分析化学]