Sequential Injection-On-line Dilution Micro-sample Introduction Technique and Its Application to Automatic Photometric Determination of Nitrite in Water Samples
摘 要
以测定环境水样中的亚硝酸盐为例,采用顺序注射技术,提出了一种智能化在线微量进样稀释分析系统(SIA系统).将测定过程中分光光度计输出的模拟电压信号,反馈至顺序注射仪,判断是否需要稀释.当获得的电压信号值小于305 mV(约相当于吸光度值0.8)时,SIA系统进入稀释程序,否则,则进入直接测定程序,两种程序均自动完成.直接测定和稀释测定的线性范围分别为1~50 μmol·L-1和50~500 μmol·L-1 NO-2.分别在NO-2浓度水平为10,200 μmol·L-1时作精密度试验,测得相对标准偏差(n=11)依次为0.7%和1.0%.该分析系统特别适合于自动分析过程中被测物质浓度变化较大而需要在线稀释的情况.
Abstract
By applying the sequential injection technique,an automatic intelligent on-line dilution micro-sample introduction system (SIA system) was proposed.Operation mode and analytical characteristic of this system was studied by its application to the photometric determination of NO-2 in water samples.The analog voltage signal output of the spectrophotometer in the course of measurement were fed back to the sequential injector,to judge whether dilution is needed or not.If the value of voltage is smaller than 305 mV (corresponding to the absorbance value of 0.8),the SIA system will proceed to the dilution program,otherwise,proceed to the direct determination program,both of which will perform automatically.Linearity ranges of the calibration curves were found ranged from 1 to 50 μmol·L-1 of NO-2 without dilution,and from 50 to 500 μmol·L-1 of NO-2 with dilution.Values of RSD′s (n=11) obtained were 0.7% (at concentration level of 10 μmol·L-1),and 1.0% (at concentration level of 200 μmol·L-1).The SIA system proposed was found to be feasible for automatic analytical process where large variation of concentration of analyte is encountered and on-line dilution is necessary.
中图分类号 O657.32
所属栏目 试验与研究
基金项目 国家自然科学基金项目(No.20575043)
收稿日期 2008/1/6
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备注刘永强(1981-),男,山东潍坊人,硕士研究生,主要从事自动分析化学的研究.
引用该论文: LIU Yong-qiang,MA Hong-bing,TAO Guan-hong. Sequential Injection-On-line Dilution Micro-sample Introduction Technique and Its Application to Automatic Photometric Determination of Nitrite in Water Samples[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(5): 501~503
刘永强,马泓冰,陶冠红. 顺序注射在线稀释微量进样技术及其在自动光度法测定水中亚硝酸盐的应用[J]. 理化检验-化学分册, 2009, 45(5): 501~503
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参考文献
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【11】GB/T 7493-1987水质 亚硝酸盐氮的测定 分光光度法[S].
【2】GUO T,BAASNER J,MCLNTOSH S.Determination of highly concentrated Na,K,Mg and Ca in dialysis solution with flow injection on-line dilution and flame atomic absorption spectrometry[J].Anal Chim Acta,1996,331:263-270.
【3】GINE M F,PACKER A P,BLANCO T,et al.Flow system based on a binary sampling process for automatic dilutions prior to flame atomic spectrometry[J].Anal Chim Acta,1996,323:47-53.
【4】REIS B F,JACINTHO A O,MORTATTI J,et al.Zone-sampling processes in flow injection analysis[J].Anal Chim Acta,1981,123:221-228.
【5】OLSEN S,RUZICKA J,HANSEN E H.Determination of hydrogen peroxide in a flow system with microperoxidase as catalyst for the luminol chemiluminescence reaction[J].Anal Chim Acta,1982,136:113-119.
【6】FANG Z,WELZ B,SPERLING M.Expasion of dynamic range of flame atomic absorption spectrometry by an efficient flow injection dilution system based on dispersion of micro-volume sample[J].Anal Chem,1993,65:1682-1688.
【7】RUZICKA J,MARSHALL G K.Sequential injection: a new concept for chemical sensors,process analysis and laboratory assays[J].Anal Chim Acta,1990,237:329-343.
【8】CERDA A,OMS M T,FORTEZA R,et al.Sequential injection sandwich technique for the simultaneous determination of nitrate and nitrite[J].Anal Chim Acta,1998,371:63-71.
【9】方肇伦.流动注射分析法[M].北京:科学出版社,1999:59-60.
【10】TAO G,FANG Z,BAASNER J,et al.Flow injection on-line dilution for flame atomic absorption spectrometry by micro-sample introduction and dispersion using syringe pumps[J].Anal Chim Acta,2003,481:273-281.
【11】GB/T 7493-1987水质 亚硝酸盐氮的测定 分光光度法[S].
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