摘要
为探究稀土氧化物中氟(F)和氯(Cl)元素含量的快速检测方法,通过全自动高温水解仪对氧化镧铈样品进行前处理,并利用氢氧根体系离子色谱仪检测吸收液中F^(-)、Cl^(-)的含量,建立了基于全自动高温水解-离子色谱法测定氧化镧铈中的F、Cl元素含量的快速检测方法,有效避免了传统前处理方法过程复杂、分析时间长、极易受人为干扰的问题。将氧化镧铈样品,在氧气流量为300 mL/min,1100℃高温燃烧水解20 min,以NaOH(15 mmol/L)作为淋洗液,经色谱柱分离,测得F^(-)与Cl^(-)在质量浓度为1.00~15.00 mg/L时,质量浓度与离子色谱峰面积呈线性关系,相关系数均为0.9999,检出限分别为0.003 mg/L和0.12 mg/L。全自动高温水解仪联用离子色谱仪检测系统对氧化镧铈中F^(-)的平均加标回收率为98.4%,标准偏差RSD为0.94%;对Cl^(-)的加标回收率为97.8%,RSD为2.9%。方法具有较高准确度及精密度,测试结果准确、可靠,满足测试要求,为稀土氧化镧铈中氟、氯元素含量的研究及相关产品的开发提供了理论基础。
To explore the rapid detection method of fluorine(F)and chlorine(Cl)in rare earth oxides,the sample of lanthanum-cerium oxide was pre-treated by automatic high temperature hydrolyzer meter,and the content of F^(-)and Cl^(-)in the absorption solution was detected by hydroxide system ion chromatograph.A rapid method for the determination of F and Cl elements in lanthanum cerium oxide based on automatic high temperature hydrolysis-ion chromatography was established.The method effectively avoided the problems of complex process,long analysis time and easy to be disturbed by human beings.The sample of lanthanum cerium oxide was hydrolyzed by combustion at an oxygen flow rate of 300 mL/min and at 1100℃ for 20 min.NaOH(15 mmol/L)was used as the eluviation solution,and separated by chromatography-column.The mass concentration of F^(-)and Cl^(-)was measured to be linearly related to the peak area of ion chromatography when the mass concentration of F^(-)and Cl^(-)was 1.00—15.00 mg/L.The corresponding correlation coefficients were 0.9999,and the detection limits were 0.003 mg/L and 0.12 mg/L,respectively.The average recovery of F^(-)in lanthanum-cerium oxide using an automatic high-temperature hydrolysis instrument combined with an ion chromatograph detection system was 98.4%,with a standard deviation RSD of 0.94%.The average spiked recovery of Cl^(-)was 97.8% and corresponding RSD was 2.9%.The method has high accuracy and precision,and the test results are accurate and reliable,which can meet the test requirements.It provides a theoretical basis for the research on the content of fluorine and chlorine in lanthanum cerium oxide and the development of related products.
作者
孙家亮
史烨弘
房胜楠
杨斐
韩鹏程
赵振
徐碧聪
李华昌
SUN Jialiang;SHI Yehong;FANG Shengnan;YANG Fei;HAN Pengcheng;ZHAO Zhen;XU Bicong;LI Huachang(BGRIMM MTC Technology Co.,Ltd.,Beijing 102628,China)
出处
《中国无机分析化学》
CAS
北大核心
2024年第5期615-621,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家重点研发计划重点专项(2021YFC2903100)。
关键词
稀土氧化物
高温水解法
离子色谱法
氟
氯
rare earth oxide
high temperature hydrolysis
ion chromatography
fluorine
chlorine
