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微波消解-电位滴定法测定不锈钢中Cr含量

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[目的]GB/T 223.11-2008测量结果准确性较高,但操作过程烦琐,耗时较长.为加快检测速率,本研究提出一种新的溶样方式.[方法]采用盐酸、硝酸、氢氟酸作为消解试剂,以微波消解的方式来溶解0.2 g样品,用电位滴定法测量不锈钢中Cr的含量.[结果]通过试验验证:最佳消解试剂为2 mL盐酸、1 mL硝酸和1 mL氢氟酸,微波消解仪的最佳消解功率为200 W,最佳保持功率时间为30 min,全自动电位滴定仪的最佳搅拌转速为40%.[结论]实现了程序化标准溶样流程控制,克服了传统滴定分析操作人员判定终点的主观误差,大幅度提高了检测的效率和准确性.
Determination of Cr Content in Stainless Steel by Microwave Digestion-Potentiometric Titration Method
[Purposes]The measurement results of GB/T 223.11-2008 have relatively high accuracy,but the operation process is cumbersome and time-consuming.In order to speed up the detection rate,this study puts forward a new dissolution method.[Methods]This paper uses HCl,HNO3 and HF as digestion reagents to dissolve 0.2 g samples by microwave digestion,and measures the content of Cr in stainless steel by potentiometric titration method.[Findings]The experimental results show that the optimal diges-tion reagents are 2 mLHCl,1 mL HNO3 and 1 mLHF,the optimal digestion power of microwave digestion instrument is 200 W,the optimal power retention time is 30 min,and the optimal stirring speed of auto-matic potentiometric titration instrument is 40%.[Conclusions]The procedure control of standard sample dissolution process is realized,and the subjective error of determining the end point by the opera-tor of traditional titration analysis is overcome,and the efficiency and accuracy of detection are greatly improved.

microwave digestionpotentiometric titration methodstainless steel

杨雪梅、谢东红、于新芝、贾旭

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航宇救生装备有限公司,湖北 襄阳 441000

微波消解 电位滴定法 不锈钢

2024

河南科技
河南省科学技术信息研究院

河南科技

影响因子:0.615
ISSN:1003-5168
年,卷(期):2024.51(23)