电感耦合等离子体原子发射光谱法测定核级锆合金中17种常量及痕量元素

Determination of seventeen major and trace elements in nuclear grade zirconium alloy by inductively coupled plasma atomic emission spectrometry

使用电感耦合等离子体原子发射光谱法对核级锆合金中4种常量元素及13种痕量元素进行测定。通过用高纯海绵锆及主合金元素进行基体匹配和选择合适的光谱线作被测元素分析线,成功地测定了核级锆合金中常量元素锡、铌、铁、铬和痕量元素铝、钴、铜、钼、镁、锰、镍、铅、硅、钽、钛、钒、钨。对NIST的360b锆合金中锡、铁、铬、镍的测定,其测定结果与标准物质证书给出的标准值相一致。对核级锆合金进行加标回收试验,结果表明,除钽的回收率偏低和铝、铅的回收率偏高外,铌、钴、铜、钼、镁、锰、硅、钛、钒、钨的回收率在92%～108%之间。本法的测定结果稳定,3天测定结果的相对标准偏差(RSD)均在6%以下,能满足西屋认证标准(RSD<10%)的要求。

Four kinds of major elements and thirteen kinds of trace elements in nuclear grade zirconium alloys were determined by inductively coupled plasma atomic emission spectrometry. The major ele- ments such as tin, niobium, iron, chromium and trace elements such as aluminum, cobalt, copper, molybdenum, magnesium, manganese, nickel, lead, silicon, tantalum, titanium, vanadium, tungsten were successfully determined by matrix matching with high-purity sponge zirconium and main alloying elements and selecting appropriate spectral line＇ as the analysis line for determined elements. Tin, i- ron, chromium and nickel in NIST 360b zirconium alloy were determined, with determined results in consistency with the standard values given in the standard substance certificate. The results for addi- tion standard recovery test of nuclear grade zirconium alloy showed that except that the recovery of tantalum was low and the recoveries of aluminum and lead were high, all the recoveries of niobium, cobalt, copper, molybdenum, magnesium, manganese, silicon, titanium, vanadium and tungsten were between 92% to 108%. The determined results of this method was stable, and the relative standard deviations （RSDs） of the determined results within three days were below 6%, that met the requirement （RSD〈10 %） of Westinghouse certification standard.