首页|铁铬液流电解液中三价铬的测定方法

铁铬液流电解液中三价铬的测定方法

扫码查看
在HG/T 4311-2012《工业氯化铬》滴定法测定三价铬含量的基础上,通过多步氧化法,将铁铬混合物中Cr3+完全氧化成Cr6+,实现了较大浓度范围内 Cr3+含量的精确稳定测试,解决了铁离子干扰;同时,对影响测定结果准确度的主要条件(蒸馏水添加量、氢氧化钠溶液添加量和盐酸溶液添加量)进行了实验验证对比分析,优化了实验条件.测定步骤主要为:先在酸性环境中用过量的氯酸钠溶液把Fe2+氧化成Fe3+,然后加氢氧化钠溶液在碱性环境下用双氧水初步把Cr3+氧化成Cr6+.此时由于部分被铁络合物包裹的Cr3+未被氧化,所以加盐酸溶液调节到合适的pH后,使被络合物包裹的Cr3+完全释出,再用双氧水完全氧化成Cr6+,然后添加硫酸溶液和磷酸掩蔽铁离子,用硫酸亚铁铵标准溶液滴定.结果表明,测定的Cr3+含量相对标准偏差为0.12%~0.51%,加标回收率为95.0%~99.2%,且测定结果与分光光度法测定结果基本一致,满足铁铬液流电池电解液中三价铬含量的测定要求.
Determination method of trivalent chromium in iron chromium flow electrolytes
The determination of trivalent chromium content was based on the titration method of"HG/T 4311-2012 Indus-trial Chromium Chloride".By using a multi-step oxidation method,Cr3+ in the iron chromium mixture was completely oxi-dized to Cr6+,achieving accurate and stable testing of Cr3+ content within a large concentration range,and solving the inter-ference of iron ions.At the same time,the main conditions that affected the accuracy of the measurement results,including the amount of distilled water,the amount of sodium hydroxide solution and the amount of hydrochloric acid,were experimen-tally verified and compared,and the experimental conditions were optimized.The main measurement steps of this method were as follows:firstly,in an acidic environment,Fe2+ was oxidized to Fe3+ with an excess sodium chlorate solution,then a so-dium hydroxide solution was added,and in alkaline environment,Cr3+ was preliminarily oxidized to Cr6+ with hydrogen perox-ide.At this point,as some of the Cr3+ encapsulated by the iron complex was not oxidized,a hydrochloric acid solution was added to adjust to the appropriate pH value to completely release the Cr3+ encapsulated by the complex.Then,hydrogen perox-ide was used to completely oxidize it to Cr6+.Then,sulfuric acid solution and phosphoric acid were added to mask the iron ions,and titrated with ammonium ferrous sulfate standard solution.The results showed that the relative standard deviation of Cr3+ determined by this method was 0.12%~0.51%,and the recovery rate of the added standard was 95.0%~99.2%.The de-termination results were basically consistent with those determined by spectrophotometry,meeting the requirements for the determination of trivalent chromium content in the electrolyte of iron chromium flow batteries.

Fe-Cr mixturetrivalent chromiumRSD

华蔓、车莹、杨合雄、温启浩

展开 >

斯瑞尔环境科技股份有限公司,广东惠州 516000

广东瑞研检测科技有限公司,广东惠州 516000

铁铬混合物 三价铬 相对标准偏差

2024

无机盐工业
中海油天津化工研究设计院 中国化工学会无机酸碱盐专业委员会

无机盐工业

CSTPCD北大核心
影响因子:0.489
ISSN:1006-4990
年,卷(期):2024.56(1)
  • 7