A FI-Electrochemoanalytical System and Its Application to In-Situ Supervising Analysis in the Process of Preparation of Calcium Citrate by Cation Exchange
摘 要
提出将流动注射电化学分析系统(离子选择电极电位检测)应用于离子交换法制备柠檬酸钠生产流程中对离子交换树脂的运行状态和从交换柱流出液中柠檬酸钙含量的自动在线监测。经试验并优化的检测条件如下:① 总离子强度调节缓冲溶液(TISAB)每升中含80 mmol Tris,175 mmol硼酸、1.0 mmol氯化钾和0.025 mmol氯化钙,此混合溶液酸度为pH 8.0;② 样品注入体积为150 μL;③ 总流量为2.26 mL·min-1;④ 混合盘管长度为120 cm(内径0.5 mm)。测定钠离子的线性范围为2.0~1 000 mmol·L-1,测定钙离子的线性范围为0.2~50.0 mmol·L-1;钠离子选择电极和钙离子选择电极的测定下限依次为1.12,0.09 mmol·L-1。分别对上述二离子的低浓度和高浓度混合标准溶液连续测定11次,测定值的相对标准偏差均小于0.7%。
Abstract
A flow-injection electrochemoanalytical system was proposed and applied to in-situ supervising analysis for content of the product and state of production in the process of preparation of calcium citrate by cation exchange. As shown by the experimental results, the optimized testing conditions were given as follows: ① a mixed solution containing 80 mmol of Tris, 175 mmol of boric acid, 1.0 mmol of KCl and 0.025 mmol of CaCl2 in 1 L of solution was used as TISAB (pH 8.0) in the analysis; ② 150 μL was taken as the volume of sample injection; ③ total flow-rate taken was 2.26 mL·min-1; and ④ length of the mixing coil taken was 120 cm (with i.d. 0.5 mm). Linearity ranges found for determination of Na+ ion and Ca2+ ion were between 2.0-1 000 mmol·L-1 and 0.2-50.0 mmol·L-1 respectively. Values of lower limits of determination found for the ISE of Na+ and Ca2+ were 1.12 mmol·L-1 and 0.09 mmol·L-1 respectively. Tests for precision were made with mixtures of standard solutions of Na+ and Ca2+ at low and high concentrations, values of RSD′s (n=11) found were all less than 0.7%.
中图分类号 O657.1
所属栏目 工作简报
基金项目 四川大学214人才振兴计划基金资助项目(0082204127067)
收稿日期 2013/5/17
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备注刘康(1988-),男,安徽铜陵人,硕士研究生,主要研究方向为化学自动化与在线监测。
引用该论文: LIU Kang,LI Yong-sheng,WANG Yue-jiao,DU Xin. A FI-Electrochemoanalytical System and Its Application to In-Situ Supervising Analysis in the Process of Preparation of Calcium Citrate by Cation Exchange[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(7): 828~832
刘康,李永生,王月姣,杜鑫. 流动注射电化学分析系统应用于离子交换法制备柠檬酸钙的在线监测[J]. 理化检验-化学分册, 2014, 50(7): 828~832
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参考文献
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【6】甘林火,翁连进,陈金河.阳离子交换树脂法制备L-组氨酸钙工艺[J].过程工程学报, 2009,9(6):1104-1108.
【7】李永生,董宜玲,吕淑清.流动注射-分光光度法测定电厂炉水中微量氯离子的试验研究[J].华北电力技术, 2003,66(2):18-22.
【8】李永生,董宜玲.用流动注射分析法测定强碱性阴离子交换树脂的交换容量[J].分析化学, 2004,32(6):787-790.
【9】李永生,郭慧.流动注射离子选择电极法自动测定阳离子交换树脂交换容量的研究[J].分析化学, 2008,36(6):805-810.
【10】周磊,赖振尧,张会生,等.同时测定血清中4种电解质的流动注射微电极串联电化学自动分析系统[J].分析化学, 2011,39(6):809-814.
【11】赖振尧,李永生,周磊,等.同时测定海水中K+、Na+、Ca2+、Cl-的流动注射离子选择电极分析[J].分析试验室, 2012,31(8):103-107.
【2】SAKHAEE K, BUHKET T, ADAMS-HUET B. Meta-analysis of calcium bioavailability: a comparison of calcium citrate with calcium carbonate[J]. Am J Ther, 1999,6(6):313-321.
【3】HERRMANN U, SCHWILLE P O, SCHMIEDL A, et al. Acute effects of calcium sodium citrate supplementation of a test meal on mineral homeostasis, oxalate and calcium oxalate crystallization in the urine of healthy humans-preliminary results in patients with idiopathic calcium urolithiasis[J]. Biomed Pharmacother, 1999,53(5/6):264-273.
【4】LEVINE B S, RODMAN J S, WIENERMAN S. Effect of calcium citrate supplementation on urinary oxalate saturation in female stone formers: implications for prevention of osteoporosis[J]. Am J Clin Nutr, 1994,60(4):592-596.
【5】HERDTWECK E, KORNPROBST T, SIEBER R, et al. Crystal structure, synthesis, and properties of tri-calcium di-citrate tetra-hydrate[J]. Z Anorg Allg Chem, 2011,637:655-659.
【6】甘林火,翁连进,陈金河.阳离子交换树脂法制备L-组氨酸钙工艺[J].过程工程学报, 2009,9(6):1104-1108.
【7】李永生,董宜玲,吕淑清.流动注射-分光光度法测定电厂炉水中微量氯离子的试验研究[J].华北电力技术, 2003,66(2):18-22.
【8】李永生,董宜玲.用流动注射分析法测定强碱性阴离子交换树脂的交换容量[J].分析化学, 2004,32(6):787-790.
【9】李永生,郭慧.流动注射离子选择电极法自动测定阳离子交换树脂交换容量的研究[J].分析化学, 2008,36(6):805-810.
【10】周磊,赖振尧,张会生,等.同时测定血清中4种电解质的流动注射微电极串联电化学自动分析系统[J].分析化学, 2011,39(6):809-814.
【11】赖振尧,李永生,周磊,等.同时测定海水中K+、Na+、Ca2+、Cl-的流动注射离子选择电极分析[J].分析试验室, 2012,31(8):103-107.
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