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首页> 外文期刊>Analytical methods >A highly selective and sensitive spectrophotometric method for the determination of selenium using 2-hydroxy-1-napthaldehyde-orthoaminophenol
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A highly selective and sensitive spectrophotometric method for the determination of selenium using 2-hydroxy-1-napthaldehyde-orthoaminophenol

机译:2-羟基-1-萘甲醛-原氨基酚的高选择性灵敏光度法测定硒

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摘要

A very simple, ultra-sensitive and highly selective non-extractive spectrophotometric method for the determination of trace amounts of selenium using 2-hydroxy-1-napthaldehyde-orthoaminophenol (HNA-OAP) has been developed. HNA-OAP reacts in slightly acidic (7 x 10(-6) to 3.5 x 10(-5) M H2SO4) aquatic media with selenium(IV) in 40% N, N-dimethylformamide (DMF) to produce a highly absorbent orange red chelate, which has an absorption maximum at 509 nm. The absorbance intensity of the metal-chelate reaches a constant value (after heating for 5 min at 45 + 5 degrees C) within 15 min and remains stable for over 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 6.30 x 10(5) L mol(-1) cm(-1) and 10 ng cm(-2) of Se, respectively. Linear calibration graphs were obtained for 0.02-7.0 mg L-1 of Se, having a detection limit of 1.0 mu g L-1, the quantification limit of the reaction system was found to be 10 mu g L-1, and the RSD was 0-2%. The stoichiometric composition of the chelate is 2 : 3 (Se : HNA-OAP). A large excess of over 60 cations, anions and complexing agents does not interfere in the determination. The method was applied successfully in the determination of selenium in several standard reference materials (alloys, steels, sediments, tea and bovine liver) as well as in some environmental waters (portable and polluted), biological samples (human blood, urine and hair), soil samples, food samples, pharmaceutical samples, solutions containing both selenium(IV) and selenium(VI) and complex synthetic mixtures. The method has high precision and accuracy (s = +/- 0.01 for 0.5 mg L-1).
机译:开发了一种非常简单,超灵敏,选择性高的非萃取分光光度法,使用2-羟基-1-萘甲醛-邻氨基苯酚(HNA-OAP)测定痕量硒。 HNA-OAP在弱酸性(7 x 10(-6)至3.5 x 10(-5)M H2SO4)水介质中与硒(IV)在40%N,N-二甲基甲酰胺(DMF)中反应生成高吸收性橙色红色螯合物,在509 nm处具有最大吸收。金属螯合物的吸收强度在15分钟内达到恒定值(在45 + 5摄氏度加热5分钟后),并在超过24小时内保持稳定。发现平均摩尔吸收系数和Sandell的敏感性分别为6.30 x 10(5)L mol(-1)cm(-1)和10 ng cm(-2)的Se。获得0.02-7.0 mg L-1的Se的线性校准图,其检出限为1.0μgL-1,发现反应体系的定量限为10μgL-1,RSD为0-2%。螯合物的化学计量组成为2:3(Se:HNA-OAP)。大量超过60种阳离子,阴离子和络合剂不会干扰测定。该方法已成功应用于多种标准参考物质(合金,钢,沉积物,茶和牛肝)以及某些环境水(便携式和污染的),生物样品(人体血液,尿液和头发)中硒的测定。 ,土壤样品,食品样品,药物样品,同时含有硒(IV)和硒(VI)的溶液以及复杂的合成混合物。该方法具有很高的准确性和准确性(对于0.5 mg L-1,s = +/- 0.01)。

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