摘要
采用自制的高温水解装置处理样品,结合离子色谱法测定了再生锌原料中氟、氯的含量。试样在1000℃高温下通入氧气与水蒸汽进行水解反应,以NaHCO3(6.0mmol/L)与Na2CO3(2.4mmol/L)的混合溶液作为淋洗液,经SH—AG-1保护柱及SH—AC-3分离柱分离,测得F-在0~10mg/L、Cl-在O~50mg/L范围内浓度与峰面积呈线性关系,相关系数分别为r=0.9998和r=0.9999,检出限分别为0.020mg/L与0.033mg/L。分析再生锌原料中氟、氯的加标回收率分别在95.70%~102.5%和96.72%~101.3%,相对标准偏差(n=11)分别在2.1%~6.6%和2.0%~5.8%。方法对再生锌原料中氟(0.010%~1.00%)和氯(0.050%~5.00%)测定,结果满意。
An analytical method for the determination of fluoride and chloride in regenerated zinc material by ion chromatography in conjunction with a self-designed high temperature-hydrolysis device was established. The samples were hydrolyzed at 1 000 ℃ in oxygen gas and steam. After hydrolysis, the solution were separated through the SH-AG-1 guard column and SH-AC-3 separation column using the mixture solution of NaHCO3 (6.0 mmol/L) and Na2CO3 (2.4 mmol/L) as the eluent. The results showed that the concentrations of fluorine ion and chloride ion had a linear correlation with their peak areas in the concentration range of 0-10 mg/L and 0-50 mg/L, respectively. And the correlation coefficients of the linear curves for fluorine ion and chloride ion were 0. 999 8 and 0. 999 9, respectively. The detection limit for fluorine ion and chloride ion were 0. 020 and 0. 033 mg/L, respectively. The standard addition recoveries for analysis of fluorine ion and chloride ion in regenerated zinc material were in the range of 95.70%--102.5% and 96.72%--101.3%, respectively. The relative standard deviation(RSD, n=11) for fluorine ion and chloride ion were in the range of 2. 1%--6.6 and 2.0 %--5.8 %, respectively. The method was applied to the determination of fluorine (0.010 % - 1.00 % ) and chlorine (0.050 % -- 5.00 % ) in regenerated zinc material with satisfactory results.
出处
《中国无机分析化学》
CAS
2016年第3期74-77,共4页
Chinese Journal of Inorganic Analytical Chemistry
基金
北京矿冶研究总院院基金项目(YJJ-2016-06)资助
关键词
离子色谱法
高温水解
再生锌原料
氟
氯
ion chromatography
high temperature hydrolysis
regenerated zinc material
fluoride
chloride