摘要
测定石膏及其制品中的氟化物和氯化物,传统分析方法过程复杂,分析速度慢,准确度及灵敏度低。本文采用超声提取技术提取样品中的氟和氯,以Na2CO3-Na HCO3作为淋洗液,色谱柱分离后通过抑制器降低背景电导,用电导检测器进行检测。通过优化样品前处理和离子色谱分离条件,在测定范围内氟和氯的含量与峰面积呈良好的线性关系（相关系数〉0.9998）,方法检测限为0.15 ng/m L（氟）和0.28 ng/m L（氯）,加标回收率为95.0%~99.7%,精密度（RSD）均小于5%（n=8）。本方法采用超声提取技术,无需净化处理即可直接分析,半小时内完成前处理,且避免了目标分析物的损失。与离子选择电极法相比,检测限由μg/m L提升至ng/m L级别。
Traditional determination of fluoride and chloride in gypsum and its products has the disadvantages of complicated pretreatment, long detection time, poor accuracy and low sensitivity. To remedy this, an ion chromatography method which can simultaneously determine the fluoride and chloride in gypsum and its products has been successfully developed. The sample was extracted firstly by ultrasonic processing and eluted by Na2CO3-Na HCO3. The solution was then separated by anion column and suppressed by self-electric chemistry suppressor.Finally,the solution was detected using a conductivity detector. By optimizing the pretreatment and separate conditions,the concentrations of the fluoride and chloride have good linear relationships with the peak area in the measured range with correlation coefficients of 0. 9999 and 0. 9998 for F-and Cl-,respectively. The proposed method yielded the detection limits of 0. 15 ng / m L and 0. 28 ng / m L for F-and Cl-,respectively,the recovery of95. 0%- 99. 7% and the RSD of less than 5%（ n = 8）. The proposed method utilizes ultrasonic extraction and avoids purification. The pretreatment can be completed in less than 0. 5 h and the loss of target analyte can be avoided. Compared with the ion selective electrode method,the detection limit of this method improves fromμg /m L to ng /m L.
出处
《岩矿测试》
CAS
CSCD
北大核心
2015年第3期330-334,共5页
Rock and Mineral Analysis
关键词
石膏及其制品
氟化物
氯化物
超声提取
离子色谱法
gypsum and its products
fluoride
chloride
ultrasonic extraction
Ion Chromatography
