Topical Problems in Elemental Analysis of Advanced Ceramic Materials

Selected prominent problems in the analysis of advanced ceramic materials are surveyed. The importance of reliability of results is discussed in the field of elemental trace- and microanalysis in view of its interaction with economy, power of detection, local resolution and speciation selectivity. Particular problems in the analysis of major constituents, trace components and microlocal distributions are based on the striking propertics of ceramics; they are exemplified. Analytical assistance must start from the beginning of the production processing, in the preparation of the powdered base materials. Determination of the stoichiometry requires high accuracy and differentiation of chemical species in bulk and surface analysis of ceramic base powders. Element trace determination by direct instrumental methods requires standard reference materials for calibration; these are currently inavailable in a sufficient variety. For optimum reliability and power of detection, element traces must be prepared in isolated form in a small excitation volume for analysis. A review on the state-of-the-art of wet-chemical combined procedures is presented. Decomposition position procedures are emphasized, due to their risk of contributing severe systematic error. Combustion in elementary fluorine is presented for decomposition of refractory materials. The performance of some direct procedures is discussed. Very efficient methods are available for element trace determinations in ceramic materials, offering high detection power. Several approaches for high-resolution local microanalysis in non-conductive ceramic materials are identified as the most promising development in the analysis of sintered compact ceramic products and devices.     

粉末压片—X射线荧光光谱法测定土壤中的铜铅锌砷锑钴铬镍等重金属元素

采用粉末压片法制样,使用ZSX PrimusⅡ型X射线荧光光谱仪,对土壤样品中与生命健康和环境污染有直接影响的重金属元素Cu、Pb、Zn、As、Sb、Co、Cr、Ni进行同时测定.选用土壤国家标准物质、以国家标准物质为基体自制校准物质绘制标准曲线,解决了相关标准不足的问题,拓宽了元素测定范围(10~20 000μg/g),重点探讨了As、Sb的测量条件.虽然As、Sb的检出限和准确测定下限较高,但对于土壤质量的评价有重要的参考意义.方法快速、简便、准确.     

XRF 熔融制样法测定铜精矿中的Cu、Fe、S、Pb、Zn、As、Bi、Mo

提出了以熔融制样法,用ＰＷ１４０４Ｘ射线荧光光谱仪测定铜精矿中Ｃｕ、Ｆｅ、Ｓ、Ｐｂ、Ｚｎ、Ａｓ、Ｂｉ、Ｍｏ,探讨了铜精矿的预氧化条件,熔融条件和玻璃化试剂地制样的影响。     

离子膜富集—XRFA法测定Cr（Ⅲ）和Cr（Ⅵ）

本文利用离子交换膜富集和分离Ｃｒ（Ⅲ）与Ｃｒ（Ⅵ），并用ＸＲＦＡ测定。     

X射线荧光光谱分析痕量稀土元素检出限的研究

本文是在原有工作基础上，对低量稀土元素的ＸＲＦＡ方法，提高灵敏度，降低检出限，作了系统论述。主要以降低背景，提高峰背比，以及提高稳定性等方面进行了研究。     

化学富集XRFA法测定岩石、土壤中稀有和稀土元素

研究了化学富集ＸＲＦＡ法测定岩石、土壤中Ｎｂ，Ｔａ，Ｚｒ，Ｈｆ，Ｔｉ，ＲＥ等微量元素的方法。化学富集采用共沉淀与离子交换结合。富集后得到的稀有和稀土元素用薄样－Ｘ荧光光谱法测定。制订了一个用明胶做分散剂制薄样的方法。稀有与稀土元素的检出限达０．０６～０．８μｇ／ｍｌ。精密度与准确度符合地球化学样品分析要求。     

XRFA聚脂薄膜-滤纸试样制备方法的改进

介绍了用于X射线荧光光谱分析（XRFA）的聚脂薄膜-滤纸试样制备改进方法及其效果实验。改进方法制备的试样具有基体效应小、样品用量少、元素分布均匀、试样反复使用不变形和便于保存等优点，特别适用于轻元素测量的试样制备。     

X荧光光谱法分析LF-VD精炼炉炉渣

采用X荧光光谱仪分析LF-VD精炼炉炉渣中TFe,CaO,MgO,Al2O3,SiO2,TiO2,MnO,P2O5等8个组分。因精炼炉渣中氧化钙含量高,我们选用了12个国家级、部级炉渣标准样品,再添加光谱纯试剂配制了数点合成标样,适应氧化钙、三氧化二铝、二氧化硅含量范围跨度较大的样品分析,同时使得分析曲线点分布均匀。用四硼酸锂作熔剂,高温熔融制样。进行了脱模剂、熔融温度及稀释比等制样条件的选择试验。采用PH模式、理论α系数校正基体的吸收增强效应,进行了方法的精密度及准确度试验。与化学法对照,各组份的定量分析结果令人满意。方法准确、快速、简便。     

X射线荧光光谱薄膜法测定多金属矿样中常量Pb,Zn,Cu,Fe,Mn

本文拟定了一个Ｘ射线荧光光谱薄膜测定常见铅、锌、铜、锰矿中０．２～ｘｘ％Ｐｂ、Ｚｎ、Ｃｕ、Ｆｅ、Ｍｎ的方法。实验考察了制片重现性和样品分解可靠性对本法结果的关键性影响，采用酸溶、钒作内标、Ｍｙｌａｒ膜制片测量。手续简便、方法精密度和准确性符合有色地质分析质量要求。     

无标样X荧光分析软件UNIQUANT在标准物质定值和未知样品鉴定中的应用

采用一种新的Ｘ射线荧光ＵＮＩＱＵＡＮＴ软件分析方法,分析了土壤标准物质和未知样品,土壤标准物质的分析结果与标准值较吻合,除氧化钠和氧化镁的相对偏差较高外,其余氧化物的相对偏差在０～１０％之间。