摘要
为建立柱后衍生离子色谱法同时测定饮用水中的IO3-、ClO2-、BrO3-和NO2-,采用高容量柱,以8.0 mmol·L-1碳酸钠作淋洗液,0.5 g·L-1邻二甲氧基联苯胺盐酸盐+5 g·L-1溴化钾 +25%甲醇+1.0 mol·L-1硝酸作衍生剂,反应温度60℃,450 nm波长处检测。方法的线性范围广、相关性好(r>0.999),相对标准偏差为0.84%-5.4%(n=6),样品加标回收率91.3%- 108.0%,检出限0.023-0.97μg·L-1。方法适用性好,可满足上述痕量阴离子试样的测定。
Ion chromatography (IC) with post-colurmn derivatization was applied to the simultaneous determination of IO3^- ClO2^- BrO3^- and NO2^- in drinking water, and its analytical conditions were studied and optimized. A high capacity anion exchange column was used in the IC separation, and a 8. 0 mmol · L^-1 Na2CO3 solution was used as eluent. A mixed solution with 0. 5 g· L^-1 o-dianisidine dihydro chloride, 5 g · L^-1 KBr, 25% methanol (vol. %) and 1.0 mol · L^-1 HNO3 was used as derivatizing reagent. Temperature of 60 ℃ was taken for the pre-column reaction, Ahsorbances were measured at 450 nm. Linear relationships were obtained in the range of 1.0-2 500μg · L^-1 for IO3^- ClO2^- BrO3^- and NO2^- ions, and in the range of 0.20-50μg· L^-1 for BROW- ion, all the correlation coefficients of which were larger than 0. 999. Detection limits (3 s) and determination limits (10 s) for these 4 anions were found in the ranges from 0. 023 to 0. 97μg· L^-1 and from 0. 1 to 3. 2 μg· L^-1 respectively. In its application to the analysis of 6 water samples, recovery tests were made by standard addition method, giving results in the range from 91.3% to 108. 0%. No significant differences were found hetween the analytical results obtained by the present method and by the conductometric method. Tests of precision were made at the concentration levels of 2. 50 μg· L^-1(for IO2^- ), 2.00 μg · L^-1 (for ClO2^-), 0.25μg · L^-1 (for BrO3^- ) and 4.00 μg· L^-1 (for NO2^-), and RSDs (n=6) obtained were 2. 1%, 2. 0%, 0.84% and 5.4% respectively. Interference of high concentrations of chloride ion was overcome in this method.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2006年第3期153-156,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)