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作 者:敬珂鸣 李永生[1] JING Kerning;LI Yongsheng(School of Chemical Engineering,Sichuan University,Chengdu 610065)
机构地区:[1]四川大学化学工程学院
出 处:《分析试验室》2020年第1期86-90,共5页Chinese Journal of Analysis Laboratory
摘 要:开发了一种基于流动注射双合并带铬黑T(EBT)-Ca(Ⅱ)络合消光光度法在线监测葡萄糖酸亚铁(Fe-Gla)合成的FIA系统,依据葡萄糖酸钙(Ca-Gla)、Fe(Ⅱ)型树脂为原料合成Fe-Gla的离子交换反应式(Ca(Ⅱ)+RFe■RCa+Fe(Ⅱ)),通过检测合成过程中的Ca(Ⅱ),实现了对Fe(Ⅱ)型树脂柱运行状态及产品中Fe-Gla含量的自动在线监测。对该系统的相关影响因素进行了优化:检测波长为660 nm、EBT浓度为280 mg/L、载流为NH3·H2O/NH4Cl(pH 12.4)的混合液。本方法测定Ca(Ⅱ)的线性范围为0~640 mg/L,对合成过程进行监测时,896 mg/L Fe(Ⅱ)、64 mmol/L H+对监测结果无影响。本方法实现了产品生产实时自动化监测分析,具有人为误差小、精度高(RSD≤0.53%,n=11)、分析速度快、试剂/试样用量少等特点。A FIA system based on flow injection double-merging zone EBT-Ca(Ⅱ)complex extinction spectrophotometry for on-line monitoring the synthesis of ferrous gluconate was developed.According to the ion exchange reaction formula of ferrous gluconate synthesized from calcium gluconate and Fe(Ⅱ)resin,that is Ca(Ⅱ)+RFe■RCa+Fe(Ⅱ),simultaneously automatic on-line monitoring of the Fe(Ⅱ)resin column and the detection of Fe-Gla content in products was realized by detecting Ca(Ⅱ)in synthesis process.The influencing factors of the system were investigated:detection wavelength was 660 nm,the EBT concentration was 280 mg/L,NH3-H2O-NH4Cl mixture(pH 12.4)was used as carriers.Under the optimized conditions,the linear range of Ca(Ⅱ)determined by this method was 0-640 mg/L.896 mg/L Fe(Ⅱ)and 64 mmol/L H+showed no effect on results of the monitoring the synthesis process.This method had the adrantages of real-time automatic monitoring of the synthesis process,small human error,high precision(RSD≤0.53%,n=11),fast analysis speed,and low reagent/sample usage.
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