电感耦合等离子体原子发射光谱法测定骨软骨一体支架中钙元素含量不确定度分析  

Uncertainty analysis of ICP-AES in measuring the content of calcium in osteochondral monolithic scaffold

作　　者：孙小莉 汤晓阳 王冬梅 吴建[2] 刘东 刘向辉 SUN Xiao-li;TANG Xiao-yang;WANG Dong-mei(Henan Institute of Medical Device Testing of Henan,Zhengzhou 450003,China)

机构地区：[1]河南省医疗器械检验所,河南郑州450003 [2]郑州大学公共卫生学院,河南郑州450001

出　　处：《中国医学装备》2019年第9期10-14,共5页China Medical Equipment

基　　金：国家重点研发计划(2018YFC0114501)“数字诊疗装备研发”;河南省科技厅2017年度科技攻关项目(172102310457)“新型骨软骨一体组织工程支架的构建”

摘　　要：目的:分析采用电感耦合等离子体原子发射光谱法(ICP-AES)测定骨软骨一体材料中钙元素含量的不确定度。方法:采用ICP-AES测定骨软骨一体材料中钙元素含量,以硝酸-氢氟酸混合酸为消解体系,采用微波消解法进行消解。并根据国家计量技术规范《测量不确定度评定与表示》,建立分析ICP-AES测定骨软骨一体材料中钙元素的数学模型,通过对测定中不确定度的标准溶液配制、试样称量、试样定容、最小二乘法拟合标准曲线、重复条件下测量及仪器等来源进行分析,合成样品含量的不确定度。结果:当取样量为0.2003 g、取置信水平95%、k=2时,测得骨软骨一体支架中钙含量为(3.08±0.29)mg/g。结论:采用ICP-AES测定骨软骨一体材料中钙元素含量的不确定度,通过分析实验过程中的质量称量、溶液体积及实验的重复性等,可确定样品含量的不确定度,不确定度的主要来源为标准溶液配制和试样定容。Objective:To analyze the uncertainty that inductively coupled plasma-atomic emission spectrometry(ICP-AES)measured the content of calcium in osteochondral monolithic materials.Methods:The content of calcium in osteochondral monolithic materials was determined by ICP-AES.The mixture of nitric acid and hydrofluoric acid was used as the digestion system and microwave digestion was adopted to implement digestion.According to National Metrology Technical Specification"Evaluation and Representation of Measurement Uncertainty",to establish and analyze a mathematical model for the determination of calcium in osteochondral monolithic materials by ICP-AES.Through analyzed the sources of standard solution preparation,sample weighing,constant volume of sample,standard curve of least squares fitting,measurement under repeated conditions,instruments and so on of uncertainty in the whole measurement process to synthesize the uncertainty of sample content.Results:When the sampled weight was 0.2003 g,the confidence level was 95%and k=2,the calcium content in osteochondral monolithic materials was(3.08±0.29)mg/g.0.288)mg/g.Conclusion:In the determination of uncertainty for calcium in osteochondral monolithic materials by adopting ICP-AES,the uncertainty of sample content can be determined through analyzes the mass weighing,solution volume,repeatability of the experiment and so on in experiment process.And the main sources of the uncertainty are the preparation of standard solution and the operation of constant volume in sample preparation.

关 键 词：钙元素 骨软骨一体支架 电感耦合等离子体原子发射光谱法 不确定度 

分 类 号：R197.39[医药卫生—卫生事业管理]