Simultaneous Determination of Fluoride, Chloride, Sulfur and Nitrogen in Imported Petroleum Coke by IC with Pyrohydrolysis
摘 要
采用高温水解-离子色谱法同时测定进口石油焦中氟、氯、硫和氮的含量。优化的试验条件如下:①高温燃烧温度为1 100℃;②氧气流量为500 mL·min-1;③水蒸气蒸发量约2 mL·min-1;④过氧化钠的用量为0.12 g。以30 mmol·L-1氢氧化钾溶液为淋洗液,抑制型电导检测器测定。4种离子的质量浓度均在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.044~0.33 mg·L-1。加标回收率为80.0%~96.0%,测定值的相对标准偏差(n=6)为2.9%~18%。
Abstract
IC was applied to the simultaneous determination of fluoride, chloride, sulfur and nitrogen in imported petroleum coke with pyrohydrolysis. The optimized conditions found were as follows:① combustion temperature of high heat was 1 100℃; ② flow of oxygen was 500 mL·min-1; ③ evaporation capacity of water vapor was about 2 mL·min-1; ④ amount of Na2O2 was 0.12 g. 30 mmol·L-1 KOH solution was used as eluant, and restraining conductance detector was used in determination. Linear relationships between values of peak area and mass concentration of the 4 ions were all kept in definite ranges, with detection limits (3S/N) of the method in the range of 0.044-0.33 mg·L-1. Values of recovery found by standard addition method were in the range of 80.0%-96.0%, and values of RSD's (n=6) were in the range of 2.9%-18%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201805006
所属栏目 工作简报
基金项目 国家质量监督检验检疫总局科研项目(2016IK140);江苏出入境检验检疫局科研项目(2016KJ21)
收稿日期 2017/5/27
修改稿日期
网络出版日期
作者单位点击查看
备注张爱平,高级工程师,主要从事光谱、色谱、电化学等方面的检验和科研工作,13814605592@139.com
引用该论文: ZHANG Aiping,WANG Hongwei,SHI Jinhui,XIONG Wei,JIANG Tao,LI Jianjun,FENG Yahui,FAN Congguang. Simultaneous Determination of Fluoride, Chloride, Sulfur and Nitrogen in Imported Petroleum Coke by IC with Pyrohydrolysis[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 520~524
张爱平,王红卫,施锦辉,熊伟,江涛,李建军,封亚辉,范崇光. 高温水解-离子色谱法同时测定进口石油焦中氟、氯、硫和氮的含量[J]. 理化检验-化学分册, 2018, 54(5): 520~524
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】程丽华,吴金林.石油产品基础知识[M].北京:中国石化出版社, 2006.
【2】姚思涵,黄婉利,王永邦,等.国内石油焦质量分析及对预焙阳极的影响[J].齐鲁石油化工, 2015,43(2):156-160.
【3】朱彬和,张培敏,郭伟强,等.膜处理-离子色谱法测定碳酸钡中的杂质阴离子[J].色谱, 2016,34(5):498-501.
【4】辛仁轩,姜镭.预富集柱-离子色谱法测定高纯水中痕量氟和氯[J].岩矿测试, 1997,16(2):150-152.
【5】王晶,冯爽,胡德新.氧弹燃烧-离子色谱法同时测定煤中氟、氯含量[J].理化检验-化学分册, 2014,50(11):1464-1465.
【6】赵悦,胡秀芳,张娟,等.高温水解-离子色谱法测定氮化硅中的氟和氯[J].理化检验-化学分册, 2016,52(4):444-447.
【7】刘敏,胡德新,王振坤,等.水蒸气蒸馏-离子色谱法测定硫化精矿中氟和氯[J].理化检验-化学分册, 2012,48(11):1321-1323.
【8】JULIANA S F P, LIANGE O D, FABIO A D, et al. Chloride determination by ion chromatography in petroleum coke after digestionby microwave-induced combustion[J]. Journal of Chromatography A, 2008,1213:249-252.
【9】胡德新,马德起,安鹏升,等.超声提取-离子色谱法测定铁矿石中水溶性氟氯溴及硝酸根[J].岩矿测试, 2012,31(2):287-290.
【10】FABIANE G A,EDUARDO D.Development of a vaporization system for direct determination of chlorine in petroleum coke by ICP-MS[J]. Microchemical Journal, 2013,109:117-121.
【2】姚思涵,黄婉利,王永邦,等.国内石油焦质量分析及对预焙阳极的影响[J].齐鲁石油化工, 2015,43(2):156-160.
【3】朱彬和,张培敏,郭伟强,等.膜处理-离子色谱法测定碳酸钡中的杂质阴离子[J].色谱, 2016,34(5):498-501.
【4】辛仁轩,姜镭.预富集柱-离子色谱法测定高纯水中痕量氟和氯[J].岩矿测试, 1997,16(2):150-152.
【5】王晶,冯爽,胡德新.氧弹燃烧-离子色谱法同时测定煤中氟、氯含量[J].理化检验-化学分册, 2014,50(11):1464-1465.
【6】赵悦,胡秀芳,张娟,等.高温水解-离子色谱法测定氮化硅中的氟和氯[J].理化检验-化学分册, 2016,52(4):444-447.
【7】刘敏,胡德新,王振坤,等.水蒸气蒸馏-离子色谱法测定硫化精矿中氟和氯[J].理化检验-化学分册, 2012,48(11):1321-1323.
【8】JULIANA S F P, LIANGE O D, FABIO A D, et al. Chloride determination by ion chromatography in petroleum coke after digestionby microwave-induced combustion[J]. Journal of Chromatography A, 2008,1213:249-252.
【9】胡德新,马德起,安鹏升,等.超声提取-离子色谱法测定铁矿石中水溶性氟氯溴及硝酸根[J].岩矿测试, 2012,31(2):287-290.
【10】FABIANE G A,EDUARDO D.Development of a vaporization system for direct determination of chlorine in petroleum coke by ICP-MS[J]. Microchemical Journal, 2013,109:117-121.
相关信息