全自动高温水解-离子色谱法测定氧化镧铈中氟、氯

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-离子的含量，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，该方法有效避免了传统前处理方法过程复杂、分析时间慢、极易受人为干扰的问题。称取0.3g氧化镧铈样品，在氧气流量为300 mL/min，1100 ℃高温下水解燃烧20 min，吸收定容为体积20mL的吸收液，以NAOH(15mmol/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 mg/L-15.00 mg/L范围内，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0.003mg/L和0.12mg/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-的平均加标回收率测定结果为98.4%，标准偏差RSD为0.94%；对Cl-的加标回收率测定结果为97.8%，RSD为2.86%。说明该方法较高准确度及精密度，测试结果准确可靠满足企业和检测机构的测试需求，为稀土氧化中氟、氯元素含量的研究及相关产品的开发提供了理论基础。

Determination of Fluorine and Chlorine in Lanthanum Cerium Rare Earth Oxides by Ion Chromatography with Automatic High Temperature Hydrolyser

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, and the content of F- and Cl- ions in the absorption solution was detected by hydroxide system ion chromatograph. A rapid method for the determination of F and Cl elements in lanthanum and cerium oxide based on automatic high temperature hydrolysis and ion chromatography was established. This method effectively avoids the problems of complicated process, slow analysis time and easy to be disturbed by human. The sample of 0.3g lanthanum-cerium oxide was weighed, hydrolyzed and burned at an oxygen flow rate of 300 mL/min at 1100 ℃ for 20 min, and the absorbent solution with a constant volume of 20mL was absorbed. NaOH(15mmol/L) was used as the eluent, and separated by chromatographic column. In the range of 1.00 mg/L-15.00 mg/L, the mass concentration of F- and Cl- has a linear relationship with the peak area of ion chromatography, and the correlation coefficients are all 0.9999. The detection limits were 0.003mg/L and 0.12mg/L, respectively. The average recovery of F- in lanthanum-cerium oxide was 98.4% and the standard deviation RSD was 0.94%. The recovery of Cl- was 97.8% and RSD was 2.86%. It is indicated that the method has high accuracy and precision, the test results are accurate and reliable to meet the testing needs of enterprises and testing institutions, and provide a theoretical basis for the study of fluorine and chlorine in rare earth oxidation and the development of related products.