摘要
氯影响钛基材料性能,目前海绵钛中氯的测定方法存在着流程长、需要的试剂多或只可定性,无法定量等问题。本文将离子色谱法用于海绵钛中氯的测定,通过海绵钛试样处理方法研究、去除钛离子效果分析、梯度淋洗程序的确定、抗干扰实验等,考察了溶剂、酸度及色谱条件对测定结果的影响,优化了色谱条件,解决了氯与钛基体难以分离的技术难题,建立了海绵钛中氯量测定的离子色谱法。研究发现,氢氟酸会影响H型阳离子交换前处理柱(简称H柱)的使用效果;处理后的海绵钛溶液需先稀释而后过滤,这样除去重金属的效果较好;硫酸-硝酸处理海绵钛在加入硝酸后须加热去除二氧化氮;随着色谱柱使用时间变长,柱效降低,Cl^(−)与SO_(4)^(2−)及NO_(3)^(−)分离度降低,可通过改变梯度淋洗程序改善分离效果。使用H柱除去钛阳离子;采用梯度淋洗程序,以KOH溶液(1.0 mL/min)淋洗液,用抑制性电导检测,外标法定量测定氯。测定线性范围为0.005~2.0μg/mL,检出限和定量检测下限分别为0.0039和0.013μg/mL,相对标准偏差(RSD)不大于5.0%,样品加标回收率94%~110%,可以分析海绵钛中0.005%~2.0%的氯,较国标GB/T 4698.25-2017的测定范围0.010%~0.40%宽,测定结果与国标光度法吻合较好,可满足海绵钛中氯含量测定的要求。
Chlorine affects the properties of titanium-based materials.At present,the problems are that the analytical process of chlorine in titanium sponge is long,many reagents are required,and it is only qualitative.In this study,ion chromatography method was used for the determination of chlorine in titanium sponge.Through the study of the treatment method of titanium sponge,analysis of titanium removal effect,determination of gradient elution procedure,anti-jamming experiments,etc.,the effects of solvents,acidity and chromatographic conditions on the results were investigated,the chromatographic conditions were optimized,and the difficult technical problem of separating chlorine from titanium matrix was solved.An ion chromatography method for the chlorine content in titanium sponge was established.It is found that①Hydrofluoric acid will affect the application effect of H-type cation exchange pretreatment column(H column for short);②The treated sponge titanium solution needs to be diluted first and then filtered,so the effect of removing heavy metals is better;③After adding nitric acid,sponge titanium treated with sulfuric acid nitric acid must be heated to drive away nitrogen dioxide;④As the use time of chromatographic column becomes longer,the column efficiency decreases,and the resolution of Cl^(-)with SO_(4)^(2-)and NO_(3)^(-)decreases.The separation effect can be improved by changing the gradient elution procedure.H column was used to remove titanium cations;The gradient elution procedure was used to elute the solution with KOH solution(1.0 mL/min),the inhibitory conductivity detection was used,and the chlorine was quantitatively determined by external standard method.The limit of detection and limit of quantification of the methods are 0.0039μg/mL and 0.013μg/mL,respectively.The relative standard deviation(RSD)is not more than 5.0%,and the recovery of standard addition is 94%~110%.It can analyze 0.005%~2.0%chlorine in titanium sponge.It is wider than that of the national standard GB/T 4698.25-2017(0.010
作者
杜米芳
常国梁
刘攀
张毅
张欣耀
李景滨
DU Mi-Fang;CHANG Guo-Liang;LIU Pan;ZHANG Yi;ZHANG Xin-Yao;LI Jing-Bin(Luo Yang Ship Materials Institute,Luoyang 471023,China;Henan Key Laboratory of Technology and Application of Structural Materials for Ships and Marine Equipments,Luoyang 471023,China;National New Material Production and Application Demonstration Platform(Advanced Marine Engineering and High-tech Ship Materials),Luoyang 471023,China)
出处
《应用化学》
CAS
CSCD
北大核心
2022年第9期1412-1420,共9页
Chinese Journal of Applied Chemistry
基金
先进海工与高技术船舶材料生产应用示范平台基金(No.TC180A6MR/2)资助。
关键词
离子色谱
海绵钛
氯
测定
Ion chromatography
Titanium sponge
Chlorine
Determination
