千瓦级微波等离子炬-原子发射光谱(MPT-AES)在油液分析中的应用

doi:10.7503/cjcu20180377

高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (12): 2651.doi: 10.7503/cjcu20180377

千瓦级微波等离子炬-原子发射光谱(MPT-AES)在油液分析中的应用

鄢雨微¹, 金伟¹(), 朱旦¹, 张涛¹, 应仰威¹, 单锦¹, 张旭晨¹, 于丙文¹, 陈挺², 刘超², 金钦汉¹

1. 浙江大学控制科学与工程学院, 智能系统与控制研究所, 杭州 310058
2. 浙江全世科技有限公司, 杭州 310053

收稿日期:2018-05-23 出版日期:2018-11-15 发布日期:2018-11-15
作者简介:
联系人简介: 金伟, 男, 博士, 高级工程师, 主要从事分析仪器方面的研究. E-mail: jinweimy@zju.edu.cn
基金资助:
国家重大科学仪器设备开发专项(批准号: 2013YQ470781)资助.

Application of Kilowatt MPT-AES in Oil Analysis^†

YAN Yuwei¹, JIN Wei^1,^*(), ZHU Dan¹, ZHANG Tao¹, YING Yangwei¹, SHAN Jin¹, ZHANG Xuchen¹, YU Bingwen¹, CHEN Ting², LIU Chao², JIN Qinhan¹

1. Institute of Cyber-systems and Control, College of Control Science and Engineering,Zhejiang University, Hangzhou 310058, China
2. Zhejiang Tracetech Technology Co. Ltd., Hangzhou 310053, China

Received:2018-05-23 Online:2018-11-15 Published:2018-11-15
Contact: JIN Wei E-mail:jinweimy@zju.edu.cn

摘要/Abstract

摘要：

采用千瓦级微波等离子炬-原子发射光谱(MPT-AES)装置对油液样品直接雾化进样分析, 对直接稀释后的润滑油中8种金属元素进行了检测, 并记录了进样时等离子体形貌的变化. 结果表明, 所有元素的校正曲线线性回归方程的R²值均优于0.995, 精密度高, 检出限接近传统的ICP-AES方法检出结果, 为MPT-AES在油液视情维修中的分析监测及在线快速监测奠定了基础. 同时还设计了一种油液在线混合进样装置, 操作方便、进样量准确, 适用于微量样品的采集和直接稀释及进样.

关键词: 微波等离子炬, 润滑油, 元素检测, 进样装置

Abstract:

The direct atomization injection analysis of oil samples by the kilowatt microwave plasma torchatomic emission spectrometry(MPT-AES) device was realized for the first time. To demonstrate the performance of this device, eight metal elements in the directly diluted lubricating oil were tested and the changes of plasma morphology during injection were recorded. The results show the high accuracy of our device with the R² values of the linear regression equations of all tested elements are greater than 0.995. Furthermore, the detection limit of this device achieves a comparable level to the traditional ICP-AES method. These results further suggest that our MPT-AES device have a great potential in the analysis and online rapid monitoring of oil-based maintenance. At the same time, an online oil mixing device was developed, which makes the operation of elements detection more convenient and the injection volume more accurate, and is especially suitable for the collection, direct dilution and injection of trace samples.

Key words: Microwave plasma torch(MPT), Lubricating oil, Element detection, Sample introduction device

中图分类号:

O657

TrendMD:

鄢雨微, 金伟, 朱旦, 张涛, 应仰威, 单锦, 张旭晨, 于丙文, 陈挺, 刘超, 金钦汉. 千瓦级微波等离子炬-原子发射光谱(MPT-AES)在油液分析中的应用. 高等学校化学学报, 2018, 39(12): 2651.

YAN Yuwei,JIN Wei,ZHU Dan,ZHANG Tao,YING Yangwei,SHAN Jin,ZHANG Xuchen,YU Bingwen,CHEN Ting,LIU Chao,JIN Qinhan. Application of Kilowatt MPT-AES in Oil Analysis^†. Chem. J. Chinese Universities, 2018, 39(12): 2651.

图/表 8

Fig.1 Schematic diagram of kilowatt MPT-AES setup

Fig.2 Comparison of plasma morphology without(A, C) and with oil sample injection(B, D)(A, B) 10 ms exposure; (C, D) 1 ms exposure.

Fig.3 Emission intensities of Cu 324.754 nm at different sampling rates

Fig.4 Emission intensities of Cu 324.754 nm at different flow rates of carrier gas

Fig.5 Emission intensities of Cu 324.754 nm at different flow rates of shielding gas

Fig.6 Relative intensities of Cu 324.754 nm at different MW forward powersS/B: signal to background ratio.

Table 1 Testing results of eight elements

Element	λ/nm	Linear regression equation	R²	RSD(%,n=11)	Detection limit
Element	λ/nm	Linear regression equation	R²	RSD(%,n=11)	MPT/(μg·mL^-1)	ICP/(μg·g^-1)
Ag	Ⅰ 328.068	y=2142.4x+221.5	0.9985	2.28	0.033	0.020^[1]
Al	Ⅰ 396.152	y=1244.0x-544.3	0.9967	2.77	0.10	0.15^[1]
Cd	Ⅰ 228.802	y=97.7x+252.4	0.9992	2.36	0.94	1.1^[30]
Cr	Ⅰ 425.435	y=1655.4x-591.4	0.9951	2.28	0.048	0.030^[1]
Cu	Ⅰ 327.396	y=3709.1x+4015.6	0.9996	1.88	0.022	0.015^[1]
Mg	Ⅱ 279.553	y=2523.5x-553.2	0.9991	2.03	0.079	0.050^[1]
Ti	Ⅱ 334.941	y=124.2x-399.3	0.9982	2.63	0.92	0.020^[1]
Zn	Ⅰ 213.856	y=271.8x+12.2	0.9996	3.45	0.35	0.015^[1]

Fig.7 Schematic diagram of online oil mixing and injection device

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千瓦级微波等离子炬-原子发射光谱(MPT-AES)在油液分析中的应用

Application of Kilowatt MPT-AES in Oil Analysis^†

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千瓦级微波等离子炬-原子发射光谱(MPT-AES)在油液分析中的应用

Application of Kilowatt MPT-AES in Oil Analysis†

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Application of Kilowatt MPT-AES in Oil Analysis^†