Abstract:Using low-pressure mercury lamp as light source, combined with the monochromator, the consistency of mercury calibration by mercury permeation tube method and mercury saturated vapor method was studied. In the mercury permeation tube experiment, the Pearson correlation coefficient between the absorption area value and the theoretical concentration was 0.9968, and the goodness of fit was 0.9936, indicating that the two groups of data were well correlated and in accordance with Lamberbeers law. Taking the absorption cross section of the experiment as the standard reference absorption cross section, it was found that the maximum concentration error was 7.45% for horizontal comparison of mercury vapor with the same concentration and vertical comparison of mercury vapor with different concentration. The above results showed that the permeation tube method is feasible, stable and accurate. When SO2 was added to the permeation tube experiment, the maximum measurement error of gaseous mercury concentration was 12.82%, indicating that SO2 interfered with the measurement of mercury absorption degree to a certain extent. In the experiment of mercury saturated vapor method, the maximum error measured with the permeation tube as the reference was within the allowable error of the standard, indicating that the two calibration methods were consistent. However, compared with the permeation tube method, the repeatability and accuracy of the mercury saturated vapor method were still insufficient, and there was a large room for improvement.
[1]吴福全, 梁柱, 王雅玲, 等. 全球大气汞排放清单研究现状 [J]. 环境监测管理与技术, 2015, 27(3): 18-21.
Wu F Q, Liang Z, Wang Y L, et al. Study on the Status of Global Atmospheric Mercury Emission Inventory [J]. The Administration and Technique of Environmental Monitoring, 2015, 27(3): 18-21.
[2]Mei Y, Li C X, Yang S, et al. A novel biosensor for the rapid and high-sensitive detection of mercury based on cleavable phosphorothioate RNA probe [J]. Sensors and Actuators: B. Chemical, 2021, 337: 129756.
[3]Maurice L, Croizier G, Le M, et al. Concentrations and stable isotopes of mercury in sharks of the Galapagos Marine Reserve: Human health concerns and feeding patterns [J]. Ecotoxicology and Environmental Safety, 2021, 215: 112122.
[4]Clarkson T W, Magos L. The Toxicology of Mercury and Its Chemical Compounds [J]. Critical Reviews in Toxicology, 2006, 36(8): 609-662.
[5]Saleh T A, Fadillah G, Ciptawati E, et al. Analytical methods for mercury speciation, detection, and measurement in water, oil, and gas [J]. Trends in Analytical Chemistry, 2020, 132: 116016.
[6]林国辉. 冷原子吸收测汞仪检出限测量不确定度分析与评定 [J]. 计量与测试技术, 2020, 47(10): 108-109.
Lin G H. Analysis and Evaluation of Uncertainty in Measurement about Detection Limit of Cold Atomic Absorption Mercury Analyzers [J]. Metrology & Measurement Technique, 2020, 47(10): 108-109.
[7]樊骅, 姚高扬, 刘伟, 等. 基于冷原子吸收分光光度法的热解析-低温等离子体脱汞技术研究 [J]. 光谱学与光谱分析, 2018, 38(7): 2279-2283.
Fan Y, Yao G Y, Liu W, et al. Experimental Study on the Mercury Contained Soil by Thermal Analytical Low Temperature Plasma Based on Cold Atomic Absorption Spectrophotometry [J]. Spectroscopy and Spectral Analysis, 2018, 38(7): 2279-2283.
[8]张磊, 戴景民. 基于连续光谱光源的单色仪标定方法 [J]. 光谱学与光谱分析, 2015, 35(8): 2348-2351.
Zhang L, Dai J M. Calibration Method for the Monochromator Based on Continuous Spectrum Light Source [J]. Spectroscopy and Spectral Analysis, 2015, 35(8): 2348-2351.
[9]郑海明, 李长朝. 高温还原法气态总汞光学监测的冷凝温度影响研究 [J]. 科学技术与工程, 2016, 16(30): 165-168.
Zheng H M, Li C Z. Study on Influence of Condensation Temperature on Optical Monitoring of Total Mercury in High Temperature Reduction Method [J]. Science Technology and Engineering, 2016, 16(30): 165-168.
[10]吴坚, 宋薇, 丁辉. 天然气以及大气中微量汞的监测方法的研究 [J]. 计量学报, 2001, 22(2): 156-160.
Wu J, Song W, Ding H. The Study on the Method for Determination of Trace Mercury in Natural Gas and Air [J]. Acta Metrologica Sinica, 2001, 22(2): 156-160.
[11]陈枳君, 曾立民. 在线大气汞分析仪渗透管标定方法研究 [J]. 环境科学学报, 2011, 31(6): 1192-1197.
Chen Z J, Zeng L M. Calibration methods for an on-line atmospheric mercury analyzer using a Permeation tube [J]. Acta Scientiae Circumstantiae, 2011, 31(6): 1192-1197.
[12]Turdukozhaeva A M. The temperature dependence of mercury saturated vapor pressure over the whole range of its liquid state [J]. Russian Journal of Physical Chemistry A, 2012, 86(4): 702-704.
[13]Evan J G, Henry W P. Photochemical Removal of Mercury from Flue Gas [J]. Industrial & Engineering Chemistry Research, 2002, 41(22): 5470-5476.
[14]郑海明, 李长朝. 基于高温还原及差分吸收光谱监测烟气汞的实验研究 [J]. 计量学报, 2017, 38(6): 780-785.
Zheng H M, Li C Z. Research on Flue Gas Mercury Based on High Temperature Reduction and Differential Absorption Spectroscopy [J]. Acta Metrologica Sinica, 2017, 38(6): 780-785.
[15]Huber M L, Laesecke A, Friend D G. The Vapor Pressure of Mercury [DB/OL]. https://doi.org/10.6028/NIST.IR.6643.
[16]郑海明, 董振良, 解东水. 基于紫外差分吸收光谱法同时监测烟气汞和二氧化硫浓度的实验研究 [J]. 中国电机工程学报, 2013, 33(35): 44-49.
Zheng H M, Dong Z L, Xie D S. Experimental study on simultaneous monitoring of mercury and sulfur dioxide concentration in flue gas based on UV Differential Absorption Spectrometry [J]. Proceedings of the CSEE, 2013, 33(35): 44-49.
[17]Marcia L H, Arno L, Daniel G F. Correlation for the Vapor Pressure of Mercury [J]. Industrial & Engineering Chemistry Research, 2006, 45(21): 7351-7361.
[18]程传箴, 李兴华. 液态纯汞的压强、体积和温度的性质 [J]. 计量学报, 1982, 3(4): 280-291.
Cheng C Z, Li X H. The PVT Properties of Liquid Mercury [J]. Acta Metrologica Sinica, 1982, 3(4): 280-291.
[19]解东水. 烟气汞在线监测校准系统的技术研究 [D]. 保定:华北电力大学, 2014.