首页|熔融制样—X射线荧光光谱法测定建盏中的常量元素含量

熔融制样—X射线荧光光谱法测定建盏中的常量元素含量

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采用X射线荧光光谱法(XRF)测定建盏中的常量元素含量(SiO2、Al2O3、Fe2O3、CaO、MgO、Na2O、K2O、TiO2),系统研究了熔剂、稀释比、脱模剂、熔融温度与时间对测定结果的影响.结果表明,当选用四硼酸锂-偏硼酸锂(67:33)作为熔剂、硝酸铵作为氧化剂、溴化锂作为脱模剂、熔剂与样品的稀释比为 10:1、熔样温度为 1050℃、熔融时间为 10 min时,实验可获得性能优异的熔片.根据熔样方法自行制备了一套参考标样,线性良好.在最优的仪器条件下,对不同标准物质进行精密度和准确度实验,相对标准偏差RSD<4%,测量结果与计算值的误差在化学分析允许差范围内.相较于传统分析方法,此方法快速、结果准确、对环境友好.
Major Elements in Jian-ware by X-ray Fluorescence Spectroscopy Method with Fusion Sample Preparation Technique
In this thesis,the content of SiO2、Al2O3、Fe2O3、CaO、MgO、Na2O、K2O and TiO2 in the Jian-ware was determined by X-ray fluorescence spectrometry(XRF),and the working conditions,such as melting agent,dilution ratio,demoulding agent,melting temperature,and time was studied.The results show that high-quality fuses were obtained under the following conditions:the lithium tetraborate-lithium metaborate mixture[m(Li2B4O7)∶(LiBO2)=67∶33]is adopted as flux,ammonium nitrate as the oxidant,and lithium bromide as the mold discharging agent.The ratio of flux to sample was 10:1 and the mixture temperature was melted at 1050℃ for 10 minutes.Under the above condition,a series of reference standards were prepared by melting,and the good linearity was observed.The detection limit,labeled recovery and precision of the method were measured to verify the accuracy of the method.In the accuracy of the artificial standard samples,we find that the relative standard deviation(RSD)was less than 4%and there were no significant difference between the measured value and the recommended value.Compared with traditional analytical methods,this method is rapid,accurate,and environmentally friendly.

Jian-wareX-ray fluorescence spectroscopy(XRF)Fusion sample preparation

杨惟喜、冯小华、甘强、陈锋、邱黎、王楠

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南平市产品质量检验所,福建 南平 354200

建盏 XRF法 熔融制样

福建省市场监督管理局科技项目

FJMS2022055

2024

市场监管与质量技术研究
福建省标准化研究院

市场监管与质量技术研究

影响因子:0.299
ISSN:2097-0870
年,卷(期):2024.(1)
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