高温水解-离子色谱法同时测定再生锌原料中氟和氯

Simultaneous Determination of Fluoride and Chloride in Regenerated Zinc Material by High Temperature Hydrolysis-Ion Chromatography

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.