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反向流动注射分光光度法测定水样中微量硅

Determination of trace silicon in water samples by reverse flow injection spectrophotometry
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摘要 提出以钼酸铵为显色剂,对甲替氨基酚-亚硫酸钠为还原剂,反向流动注射分光光度法测定水样中硅。对流动注射的技术条件进行了优化,结果为:以硫酸-草酸作为参比液,进样环体积为250μL,混合试样和进行反应的反应圈长度均为3m,试样溶液流速为0.85mL/min,参比液、显色液和还原剂的流速均为0.40mL/min。优化试验条件下,得到良好的校准曲线,线性范围25~1500ug/L,检测限为21.3ug/L。对200ug/L的Si(Ⅳ)标准溶液进行16次平行测定,得到相对标准偏差为2.2%。方法用于水样中硅的测定,加标回收率为95%~105%。 The determination of silicon in water by reverse flow injection spectrophotometry was developed using ammonium molybdate as color agent and methylaminophenol-sodium sulfite as reducing agent. The optimized technical conditions of flow injection were as follows: sulfuric acid-oxalic acid as reference solution; the sampling loop volume, 250μL; the lengths of reaction coils for mixing sample and carrying out reaction, both 3 m; the flow rate of sample solution, 0.85mL/min; the flow rate of reference solution, color agent and reducing agent, all 0.40 mL/min. Under these optimized experimental conditions, a good calibration curve could be obtained with the linear range of 25--1500 /_tg/L and detection limit of 21.3 μg/L. 200 μg/L Si (Ⅳ) standard solution was determined for 16 times, with the RSD of 2. 2 %. The recovery of standard addition for actual water sample was 95 %-- 105 %.
作者 肖凯 张新申
出处 《冶金分析》 CAS CSCD 北大核心 2009年第2期65-68,共4页 Metallurgical Analysis
基金 国家863资助项目(2002AA639290)
关键词 反向流动注射分析 分光光度法 参比液 reverse flow injection analysis spectrophotometry silicon reference solution
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