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  

Simultaneous Determination of Fluoride,Chloride,Sulfur and Nitrogen in Imported Petroleum Coke by IC with Pyrohydrolysis

作　　者：张爱平[1] 王红卫[1] 施锦辉[1] 熊伟[1] 江涛[1] 李建军[2] 封亚辉[2] 范崇光[3] ZHANG Aiping;WANG Hongwei;SHI Jinhui;XIONG Wei;JIANG Tao;LI Jianjun;FENG Yahui;FAN Congguang(Nantong Entry and Exit Inspection and Quarantine Bureau, Nantong 226004, China;Jiangsu Entry and Exit Inspection and Quarantine Bureau, Nanjing 210001, China;College of Chemistry and Chemical Engineering, Nantong University, Nantong 226000, China)

机构地区：[1]南通出入境检验检疫局,南通226004 [2]江苏出入境检验检疫局,南京210001 [3]南通大学化学化工学院,南通226000

出　　处：《理化检验（化学分册）》2018年第5期520-524,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：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)

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2mL·min^(-1);(4)过氧化钠的用量为0.12g。以30mmol·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0.044~0.33mg·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%。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 Na2 O2 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（3 S/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%.

关 键 词：离子色谱法 高温水解 石油焦 氟 氯 硫 氮 

分 类 号：O657.7[理学—分析化学]