电厂常规水分析化学的仪器自动化技术研究及应用
发布时间：2019-05-20 04:28
【摘要】：本论文提出了TPTZ-Fe~(2+)显色体系-流动注射分光光度法测定水汽中的痕量铁含量。通过将流动注射分析仪与紫外监测器、高温自动加热密闭消解模块联用,利用TPTZ与二价铁显色反应的方法,实现了全封闭实时在线测定电厂水汽中的总铁含量。实验研究了试剂条件优选和水样消解条件优选以及p H值对系统测定的影响,完成了消解、化学反应、检测三大块实验台搭建并进行了初步应用,结果表明本方法所测定电厂水汽中的总铁准确度较高。1、试剂条件优选。(1)总铁浓度在0-80mg/L范围内,抗坏血酸浓度为10mg/L,TPTZ浓度为40mg/L。高量程铁在优选时分成了两个阶段,总铁浓度在0-1mg/L范围内时,抗坏血酸浓度为20mg/L,TPTZ浓度为80mg/L;总铁浓度在1-3.5mg/L的范围内时,抗坏血酸浓度为40mg/L,TPTZ浓度为240mg/L。配制100mg/L硫酸铁铵母液所用HCl浓度优选。(2)测定试样铁离子浓度范围在0-100ug/L,选择用4mol/L或者5mol/L盐酸,测定试样铁离子浓度大于100ug/L时,选择1mol/L的盐酸。2、p H值对系统测定的影响。采用不同方法探索了待测试样酸度对灵敏度的影响,实际检测过程中应使试样p H值在最适宜的范围内,当检测试样的总铁含量大于100ug/L时可以适当拓宽p H值范围,在2.3-3.5之间,当含量为小于等于100ug/L时则尽量将检测试样p H值控制在2.3-3之间。3、水样消解条件优选。90℃水浴加热条件下,加0.1m L消解液,消解10min即可消解完全。在此实验数据的基础上确定了在线消解实验停留时间、加热模块温度、泵管内径、泵速等条件,优选出的停留时间10min,对应的蠕动泵挡位为1挡,泵速为5r/min,在此挡位下总流量为1m L/min,冷却盘管可以将消解后的高温液体冷却到室温。泵管径为酸路管径为0.38mm,水样路管径为2.58mm。4、将消解、化学反应、检测三大块实验台搭建完整,并利用该系统对张家口宣化热电启动机组的炉水实际水样进行测定,与哈希标准测定方法作比较,相对误差在2%左右,结果显示本方法所测定电厂水汽中的总铁准确度较高。
[Abstract]:In this paper, a TPTZ-Fe~ (2) color system-flow injection spectrophotometry was proposed for the determination of trace iron in water vapor. By combining the flow injection analyzer with UV monitor and high temperature automatic heating closed digestion module, the total iron content in water vapor of power plant was determined on-line by using the method of color reaction of TPTZ with divalent iron. The effects of reagent condition optimization, water sample digestion condition optimization and pH value on the systematic determination were studied experimentally. the digestion, chemical reaction and detection three experimental platforms were built and applied. The results show that the accuracy of the determination of total iron in water vapor of power plant is high. 1. The reagent conditions are optimized. (1) in the range of 0-80mg/L, the concentration of ascorbic acid is 10 mg 路L and the concentration of TPTZ is 40 mg 路L ~ (- 1). The high range iron was divided into two stages. When the total iron concentration was in the range of 0-1mg/L, the concentration of ascorbic acid was 20 mg 路L and the concentration of TPTZ was 80 mg 路L, and the concentration of ascorbic acid was 20 mg 路L ~ (- 1) and the concentration of TPTZ was 80 mg 路L ~ (- 1). When the total iron concentration is within the range of 1-3.5mg/L, the concentration of ascorbic acid is 40 mg 路L and the concentration of TPTZ is 240 mg 路L ~ (- 1). The concentration of HCl used in the preparation of 100mg/L ammonium iron sulfate mother liquor was optimized. (2) the concentration range of iron ion in the sample was 0 渭 g 路L ~ (- 1), and the concentration of iron ion in the sample was higher than 100ug/L when the concentration of iron ion was 0 渭 g 路L ~ (- 1), 4mol/L or 5mol/L hydrochloric acid was selected. The effect of hydrochloric acid. 2, pH value of 1mol/L on the determination of the system was selected. The influence of acidity on the sensitivity of the sample to be tested was explored by different methods. The pH value of the sample should be made in the most suitable range in the actual detection process, and the range of pH value could be widened appropriately when the total iron content of the sample was greater than 100ug/L. In the range of 2.3 鈮，
本文编号：2481351
[Abstract]:In this paper, a TPTZ-Fe~ (2) color system-flow injection spectrophotometry was proposed for the determination of trace iron in water vapor. By combining the flow injection analyzer with UV monitor and high temperature automatic heating closed digestion module, the total iron content in water vapor of power plant was determined on-line by using the method of color reaction of TPTZ with divalent iron. The effects of reagent condition optimization, water sample digestion condition optimization and pH value on the systematic determination were studied experimentally. the digestion, chemical reaction and detection three experimental platforms were built and applied. The results show that the accuracy of the determination of total iron in water vapor of power plant is high. 1. The reagent conditions are optimized. (1) in the range of 0-80mg/L, the concentration of ascorbic acid is 10 mg 路L and the concentration of TPTZ is 40 mg 路L ~ (- 1). The high range iron was divided into two stages. When the total iron concentration was in the range of 0-1mg/L, the concentration of ascorbic acid was 20 mg 路L and the concentration of TPTZ was 80 mg 路L, and the concentration of ascorbic acid was 20 mg 路L ~ (- 1) and the concentration of TPTZ was 80 mg 路L ~ (- 1). When the total iron concentration is within the range of 1-3.5mg/L, the concentration of ascorbic acid is 40 mg 路L and the concentration of TPTZ is 240 mg 路L ~ (- 1). The concentration of HCl used in the preparation of 100mg/L ammonium iron sulfate mother liquor was optimized. (2) the concentration range of iron ion in the sample was 0 渭 g 路L ~ (- 1), and the concentration of iron ion in the sample was higher than 100ug/L when the concentration of iron ion was 0 渭 g 路L ~ (- 1), 4mol/L or 5mol/L hydrochloric acid was selected. The effect of hydrochloric acid. 2, pH value of 1mol/L on the determination of the system was selected. The influence of acidity on the sensitivity of the sample to be tested was explored by different methods. The pH value of the sample should be made in the most suitable range in the actual detection process, and the range of pH value could be widened appropriately when the total iron content of the sample was greater than 100ug/L. In the range of 2.3 鈮，
本文编号：2481351
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