摘要
采用自制高温水解装置,建立了高温水解前处理铁矿石样品,离子色谱法同时测定其中氟和氯含量的方法。考察了称样量、水解温度和时间、催化剂种类和用量、氧气和水流量对水解效果的影响,确定了最佳的高温水解分解条件:样品量为0.5g;水解温度为1 100℃;水解时间为30min;样品与水解催化剂V_2O_5的质量比为1∶1;氧气流量为300mL/min;蠕动泵流量为1.5mL/min;采用两组水作为吸收剂。氟和氯的质量浓度在1.00~20.00μg/mL范围内,质量浓度与其峰面积呈线性,校准曲线的线性相关系数R^2均大于0.999 5。方法中氟和氯的检出限分别为3.7和4.9μg/g。按照实验方法测定铁矿石标准样品中氟和氯,结果的相对标准偏差(RSD,n=6)为1.0%~2.1%,并与认定值相吻合。
The iron ore sample was pretreated by self-made pyrohydrolysis device. The simultaneous deter- mination method of fluorine and chlorine in iron ore by ion chromatography was established. The influence of sample mass, hydrolysis temperature and time, catalyst type and dosage, oxygen and water flow rate on hydrolysis effect was investigated. The optimal temperature hydrolysis conditions were obtained： the sam- ple mass was 0. 5 g, the hydrolysis temperature was 1 100 ℃, the hydrolysis time was 30 min, the mass ratio of sample and catalyst （V2O5） was 1 ： 1, the oxygen flow rate was 300 mL/min, and the peristaltic pump flow rate was 1.5 mL/min. Two groups of water were used as absorbent. The mass concentration of fluorine and chlorine in range of 1.00-20.00 μg/mL was linear to the peak area. The linear correlation coef- ficients （R^2） of calibration eurves were higher than 0. 999 5. The detection limit of fluorine and chlorine in proposed method was 3. 7μg/g and 4. 9 μg/g, respectively. The proposed method was applied to the de- termination of fluorine and ehlorine in iron ore certified reference materials. The relative standard devia- tions （RSD, n=6） were between 1.0% and 2. 1%. The determination results were consistent with the certified values.
出处
《冶金分析》
CAS
CSCD
北大核心
2016年第6期23-28,共6页
Metallurgical Analysis
基金
河北省科技条件建设项目(12966912D)
河北省科技计划项目(13273707)
河北省唐山市科技计划项目(14130238B)
关键词
铁矿石
高温水解
离子色谱法
氟
氯
iron ore
pyrohydrolysis
ion chromatography
fluorine
chlorine
