利用自行研制的复合流动比色装置与单光束分光光度计相结合,建立了一种新的流动注射吸光光度检测技术.基于pH=10的Na3B4O7—NaOH缓冲溶液中,显色剂(HCPCF)能与样品中的Ge(V)形成有色络合物(λmax =630 nm).一次注入样品,在样品光束同时产生两峰一谷三个拐点(A1A2A3)的光谱吸收曲线.依据光度吸收净值(ΔA=A1 +A2 +A3)与样品中Ge(V)含量的关系进行定量分析.分析性能对比表明,显色体系稳定性、选择性和方法的灵敏度均优于普通FIA法.每个拐点的响应信号都可用于定量分析.信息量丰富,灵活多样,完全符合定量分析要求.而且分析灵敏度提高了2.3倍.进样频率为130次/h,用于煤矿石中微量锗测定,加标回收率均在100.7~101.9之间,相对标准偏差(RDS%,n=8)小于1.3%.回收率在99.7~101.4之间.
This paper was developed composite flow colorimetricwith a single beam spectrometer combining spectrophotometer to establish a new flow injection absorption spectrophotometric testing technology. Based on the pH = 10 NaaB407-NaOH buffer solution, chromogenic reagent (HCPCF) with the Ge ( V ) of samples form colored complex ( Amax = 630nm). One time injection detection at the same time the samples produced three inflection point (A1 A2 A3 ) of two peaks and one valley spectrum absorption curve. Based on photometric net ( A A = A1 + A2 + A3 ) and Ge ( V ) content of samples analysis of the relationship of capacity. Comparative analytical performance shows that the stability of color system and the selectivity and sensitivity of method are better than ordinary FIA method. For each inflexion point response signal can be used for quantitative analysis. Rich information, flexible and diverse, complete with quantitative analysis requirements. And the sensitivity analysis is improved by 2.3 times. Sample frequency for 130 times/h,used trace deter mination of Ge in coal mine stone,is prevented, the recovery of standard addition is in between 100.7 and 101.9, and relative standard deviation ( RDS % ,n =8) less than 1.3%. Recovery from 99.7 to 101.4.