基于流动注射分析测定催化剂共浸液中高浓度CoO的研究

发布时间：2018-06-29 11:56

本文选题：钴离子 + 催化剂　；参考：《分析试验室》2017年12期

【摘要】：为了监测钴钼催化剂浸渍液中高浓度Co(Ⅱ)含量,基于Co(Ⅱ)/KSCN反应体系,建立了一种能测定上述离子的流动注射分光光度系统。研究发现:Co(Ⅱ)与KSCN络合物是由K_2Co(SCN)_4和K_4Co(SCN)_6构成,利用第二种物质可以定量Co(Ⅱ);共浸液实样在碱性或强酸性条件下能形成稳定均一的溶液,而在中性和弱酸性条件下则会出现大量溶质析出的问题。利用硫酸将样品酸化至pH≈0.38,可以实现实样的测定。另外,本研究对相关影响因素进行了优化,得到的测定条件为:显色剂由37.5%(w/V)KSCN和0.1 mol/L Na Ac-HAc(pH 5.8)组成,载流为1.0 mol/L硫酸,系统出口总流量为2.0 m L/min,样品定量环体积为90μL,显色剂定量环体积为220μL,测定波长为620 nm。本方法的线性范围5.0~50.0 g/L,检出限1.3 g/L。系统的RSD1.2%(n=11),回收率为96.0%~102.7%,分析速度为20样/h。
[Abstract]:In order to monitor the content of high concentration Co (II) in the impregnated solution of Co Mo catalyst, a flow injection spectrophotometric system is established based on the Co (II) /KSCN reaction system. The study shows that the Co (II) and KSCN complexes are composed of K_2Co (SCN) _4 and K_4Co (SCN) _6, and second substances can be used to quantify Co (II). A stable homogeneous solution can be formed under alkaline or strong acidic conditions, while a large number of solute precipitates appear in neutral and weak acidic conditions. The sample can be acidified to pH 0.38 by sulfuric acid. In addition, the related factors are optimized and the conditions for the determination are 37.5% (w/V) of chromogenic agent. KSCN and 0.1 mol/L Na Ac-HAc (pH 5.8) are composed of 1 mol/L sulfuric acid, the total flow rate of the system is 2 m L/min, the quantitative ring volume of the sample is 90 micron, the volume of the chromogenic agent is 220 mu L, the determination of the wavelength is 620 nm., and the detection limit is 1.3. 20 kinds of /h.
【作者单位】：四川大学化学工程学院;
【分类号】：O643.36;O657.3

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