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1、成都理工大学 硕士学位论文 煤中砷、汞和氯的分析方法及燃煤中砷、汞的迁移规律研究 姓名：凤海元 申请学位级别：硕士 专业：分析化学 指导教师：苏庆平;龙小玲 20100501 摘 要 I 煤中砷、汞和氯的分析方法及燃煤中砷、汞的 迁移规律研究 煤中砷、汞和氯的分析方法及燃煤中砷、汞的 迁移规律研究 作者简介：凤海元，男，1984 年 12 月生，师从成都理工大学苏庆平副教 授，龙小玲高工，2010 年 6 月毕业于成都理工大学分析化学专业，获得理学硕 士学位。 摘 要 摘 要 正确地表示煤中微量元素的含量，是评价煤中潜在有害微量元素的环境效 应的重要依据，一直以来都是煤炭科学领域里的难题。本课
2、题为导师和煤碳科 学研究总院北京煤化工研究分院合作的国家横向科研课题煤中砷、汞含量分 级与限值标准研究和国家科技支撑计划项目动力配煤及优质化示范工程 中的一部分，分析研究煤中砷、汞和氯等有害微量元素的迁移规律及其限值。 本文重点革新和解决了煤炭样品中微量、痕量有害元素砷、汞和氯的分析 测试方法问题。长期以来，原子荧光技术应用于煤中砷、汞的测试问题， 文献 尚未见报道。本文针对地域不同的煤炭样品，应用原子荧光分析技术，全面实 验对比了多种溶矿方法对煤中砷、汞的浸出情况，拟定了原子荧光法测定煤中 砷、汞的分析流程，并应用于大量生产实践，充分验证了方法的可行性。 针对煤中砷、汞的形态分析，论文创新性
3、的开展了提取序列的研究，表明 形态分析结果受提取剂极性的强弱和提取顺序的影响很大，尤其是本实验中硫 化态和有机态受提取序列变化非常显著， 分别在不同的提取序列中达到最大值， 这一研究结果为形态分析工作者提供了有悖常规的研究思路和思考。 通过大量条件试验对比，确立了简单、快速、成本低廉的比浊法进行煤中 低氯的测定，经与权威的成都煤炭产品质量监督检验站提供的高温燃烧水解- 电位滴定法测氯结果对照， 误差均在不确定度 0.003 %范围以内， 符合痕量分析 要求。同时提供了一种视觉新颖的分析方法，即应用回归分析法探讨煤中氯与 钾、钠、钙、镁等阳离子的赋存关系，结果表明，线性关系不显著，有悖相关 论文
4、报告。 论文还实验探索了煤中砷、汞的燃烧挥发分布规律，结果表明，汞的挥发 性远强于砷，汞于 800时已经挥发完全，而砷则须达到 1200才能够挥发完 全，各因素对汞的挥发率影响大小依次为：燃烧温度燃烧时间煤粒径空 气流量称样量；各因素对砷的挥发率影响大小依次为：燃烧温度称样量 成都理工大学硕士学位论文 II 燃烧时间空气流量煤粒径。同时，经实验确立了最佳燃烧条件为：称样量 为 1.0000 g,燃烧时间 1 h，燃烧温度 1000，吸收介质 5%王水。 论文根据燃烧试验装置实行了革新，使用体积较小，携带方便，调控自如， 压力稳定的电磁式空气泵代替复杂的氮、氧组合钢瓶，使实验成本大大降低， 仪器
5、组装更加简捷，操作更加方便，有利于推广普及。 关键词：原子荧光 形态分析 迁移规律 溶矿方法 比浊法 Abstract III The Methods of Instrumental Analysis on Arsenic, Mercury , Chlorine in Coal and the Study on the law of migration of Arsenic, Mercury from coal combustion Introduction of the author:Feng haiyuan, male, was born in December, 1984 whose t
6、utors were Professor Su qingping and Long xiaoling. He graduated from Chengdu University of Technology in analytical chemistry major and was granted the Master Degree in June, 2010. Abstract Content of trace elements in coal could be showed correctly that this is according to evaluate the environmen
7、tal effects on trace elements which is harmful for potentially.And also,this is difficult to reseach in the field of coal science. environmental around the world at present.The thesis was supported by horizontal research projects the Classification and the Limits of arsenic and mercury in standars a
8、bout coal and the national science and technology support projectsSteam coal blending and Quality demonstration projectfrom Beijing Research Institute of Coal Chemistry which is a part of China Coal Research Institute that study on the law of migration and the limits of arsenic,mercury and in coal.
9、In this paper,the methods of instrumental analysis on arsenic, mercury and chlorine in Coals could be innovated and overcomed.The methods of instrumental analysis on arsenic and mercury by atomic fluorescence spectrometry were not reported as yet.Many dissolution methods and the leaching results of
10、arsenic and mercury in the coal samples from different regions were contrasted.And the analysis which could be applied in practice mostly have be made out that the methods of instrumental analysis are feasible. By studying the extraction sequence innovatively, this experiment aimed at the speciation
11、 analysis that could be vulnerable to the polarity of extracting agent and the proper order of extraction seriously, especially in this experiment,the influence of extraction sequence on sulfide formation and organic formation in obvious,and the leaching rate respectively reaches maximum value in di
12、fference extraction 成都理工大学硕士学位论文 IV sequence.The study coulde provided for a serious train of thought and consider the Analytical Chemists who study the speciation analysis. Through large amount of lab experiments,a simplified, rapid and costless turbidimetry for the determination of low-chlorine co
13、ntent in coal has been developed.By comparison with experimental data that is tested for combustion hydrolysis-potentiometric titration provided by Sichuan Province the sources of coal quality monitoring,the error is content with the uncertainty of 0.003 % that is satisfied for analysis on the trace
14、 amounts of low-chlorine in coal. In addition,the forms of chlorine with potassium,sodium,calcium and magnesium has been discussed by analysis of regression which is novel for visual.The results shows that their relationship are not close as according to reports in the literature differently. In thi
15、s experiments, the distribution of arsenic and mercury in volatility were probed into,and the results show that arsenic and mercury are all volatile elements, but mercury is be more volatily than arsenic.When the mercury volatiled completely at the low temperature of 500 ,arsenic volatiled completel
16、y at the temperature of 1200 . The factors affecting the volatilization of mercury were in the order:the combustion temperatureburning timecoal particle sizethe flow of airsample weight;The factors affecting the volatilization of arsenic were in the order:the buring temperaturesample weightburning timethe flow of airparticle size. In order to study arsenic and mer
