光谱学与光谱分析, 2018, 38 (6): 1824, 网络出版: 2018-06-29  

盐浴复合热处理氰酸根顺序注射研究和测定

Study and Determination the Concentration of CNO-Ion of the QPQ with the Sequential Injection Spectrophotometric Method
作者单位
1 西南大学工程技术学院, 重庆 400715
2 重庆电子工程职业学院, 重庆 401331
3 重庆大学微系统研究中心, 重庆 400044
摘要
一种新的金属表面改性(quench-polish-quench, QPQ)盐浴复合热处理技术能大幅度提高金属表面的耐磨性和抗蚀性。 氮化盐中氰酸根离子(CNO-)的含量是QPQ工艺质量控制的重要参数。 研究采用分光光度和顺序注射法对氰酸根离子(CNO-)含量进行定量分析。 研究了将CNO-离子通过高温高压定量转化成铵根离子(NH+4), 再依据水杨酸分光光度法, 通过对NH+4的测定, 间接实现氰酸根离子含量的检测, 选取697 nm为定量分析谱线, 实验结果表明检测的线性范围0.02~0.6 mg·kg-1, 最低检出限为0.018 mg·kg-1, 基于顺序注射法实现QPQ工艺中CNO-含量全自动原位检测。 测量均值相对误差和相对标准方差分别为1.31%和0.92%, 测定结果满足要求, 精确度高和重复性好, 优于传统化学滴定法, 为盐浴复合热处理技术中氮化盐氰酸根的全自动原位测定仪器开发提供了理论和技术支持。
Abstract
Anew technology of metal surface modification-QPQ (Quench-Polish-Quench) Salt bath compound heat treatment technology can improve theabradability and anticorrosion of metal surface. The CNO-ion plays a very important role in the quality control of QPQ technology. A sequential injection spectrophotometric method is proposed for the determination of CNO-ion. In addition, the indirect detection method of converting CNO-ion into ammonium ion (NH+4) in the condition of high temperature and high pressure is studied; a 697 nm line is selected as the characteristic wavelength. The measuring range of this experiment setup is 0. 02~0. 6 mg·kg-1, and the limit of detection (LOD) is 0.018 mg·kg-1. Based on the sequential injection, the setup can completely automatic on-situ test the concentration of CNO-ion in the quench-polish-quench (techniques for heat treatment of salt bath) process. Measure mean relative error and relative standard variance is 1.31%, 0.92% respectively. Compared with the traditional standard measurement method, a high precision and good repeatability result meets the requirements, which provides theoretical and technical support for the development of the fully automatic in-situ measurement instrument for the treatment of the salt bath compound heat treatment technology.

武新, 李光林, 温志渝. 盐浴复合热处理氰酸根顺序注射研究和测定[J]. 光谱学与光谱分析, 2018, 38(6): 1824. WU Xin, LI Guang-lin, WEN Zhi-yu. Study and Determination the Concentration of CNO-Ion of the QPQ with the Sequential Injection Spectrophotometric Method[J]. Spectroscopy and Spectral Analysis, 2018, 38(6): 1824.

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