反射式流通池顺序注射光度检测系统的研制

Studies on Sequential Injection Spectrophotometric System Using A Reflective Flow Cell for Process Analysis

提出一种反射式流通池用于过程分析光度检测系统 ,可以明显地抑制折光指数效应产生的干扰。以发光二极管为光源 ,采用多股光纤分别与流通池 ,光源 ,检测器耦合 ,实现对透射后反射回的光谱检测。以Cl- Hg(SCN) 2 Fe(Ⅲ )反应显色体系为模型对系统的实验参数进行了优化。讨论了试剂注入量、进样量、载流流速、试剂注入次序等参数对检测结果的影响。方法的线性范围为 0～ 10 0mg·L-1(相关系数r =0 998) ;分析精度 (RSD ,n =11)为 1 5 % ;检出限为 1 2mg·L-1;分析速度为 30个样·h-1;对自来水和海水的回收率分别为 95 %和 10 4 %。

A reflective flow cell was developed and coupled to a sequential injection system and optical fiber photometric detection system based on emitting diode light source. A multistrand bifurcated optical fiber was coupled with incident light, detector and flow cell. Optical fibers were used to carry light from the electronics unit to a reflective flow-through cell and back. The liquid flow path through the cell is linear with a large exit aperture such that bubbles are not trapped in the optical path. The optical arrangement is such that the incident light crosses the liquid flow orthogonally and is reflected back to the receiver fiber. This arrangement reduces the reflective index sensitivity by an order of magnitude relative to a conventional flow cell. The cell showed good immunity to refractive index and air bubble effects. The chromogenic reaction of chloride ion with mercury thiocyanate-iron (III) was used as a model reaction to optimize the experiment system and check the optical system. The reflectance of the reaction was monitored with blue emitting diode. The, linear range was 0-100 mg(.)L(-1) Cl-. A detection limit (3sigma) of 1.2 mg(.)L(-1), precision of 1.5% (n = 11), and a throughput of 30 samples per hour were achieved.