管式炉燃烧-离子色谱法测定车用柴油中的硫
王硕123,段卫宇123,曹聪123,张斌123,杨哲元123,薛绿林123,邱连强12,邱兆军1
1.辽宁省产品质量监督检验院,沈阳 110144; 2.国家石油产品质量监督检验中心(沈阳),沈阳 110144; 3.辽宁省工业润滑油液监测工程实验室,沈阳 110144
Determination of sulfur in vehicle diesel oil by tube furnace combustion with ion chromatography
王硕123,段卫宇123,曹聪123,张斌123,杨哲元123,薛绿林123,邱连强12,邱兆军1
1. Liaoning Inspection Institute of Product Quality Supervision, Shenyang 110144, China; 2. National Center of Petroleum Quality Supervision Inspection (Shenyang), Shenyang 110144, China; 3. Liaoning province industrial lubricating oil monitoring engineering labotatory, Shenyang 110144, China
摘要:建立一种管式炉燃烧-离子色谱法测定车用柴油中硫含量的方法。分别对取样量、涂布形状、管式炉的加热温度和加热速率、吸收液等影响因素进行了分析。样品经管式炉燃烧,在吸收液中转化成硫酸根离子,选用Dionex IonPac AS18 阴离子分析柱,以10 mmol/L NaOH 溶液作为淋洗液,流量为1.0 mL/min,进样体积为20 μL,以抑制电导检测器测定硫酸根离子的含量。硫酸根离子的质量浓度在0.01~5.00 mg/L 范围内与色谱峰面积呈良好的线性关系,相关系数为0.999 8,方法检出限(S/N=3) 为0.003 6 mg/L。测定结果的相对标准偏差小于5%(n=6),样品的平均加标回收率为96.63%~99.33%。该方法操作简便、快速,可用于车用柴油产品中总硫含量的测定。
Abstract:A method for the determination of sulfur in vehicle diesel oil by tube furnace combustion with ion
chromatography was established. The influence factors of sampling volume, coating shape, heating temperature, heating rate
and absorbing liquid of tube furnace were analyzed. The sample was burned by a tube furnace and changed into solution as
SO4
2-. The Dionex IonPac AS18 anion analysis column was used. 10 mmol/L NaOH solution was used as the eluent, with
the flow rate of 1.0 mL/min and the injection volume of 20 μL. Sulfate ion was determined by suppressed conductivity
detector. The mass concentration of sulfate ion had a good linear relationship with the peak area of the chromatographic
peak in the range of 0.01-5.00 mg/L, and the correlation coefficient was 0.999 8, the detection limit(S/N=3) was 0.003 6
mg/L. The relative standard deviations of the determination results were less than 5%(n=6), and the average recoveries of
the samples were 96.63%-99.33%. The method is simple and rapid, and it can be used for the determination of total sulfur
content in vehicle diesel oil.
关键词:管式炉燃烧;离子色谱法;车用柴油;硫
Keywords:tube furnace combustion; ion chromatography; vehicle diesel fuel; sulfur
基金:辽宁省自然科学基金指导计划、辽宁省自然科学基金计划重点项目(20170520108)
本文引用格式:
王硕,段卫宇,曹聪,等. 管式炉燃烧- 离子色谱法测定车用柴油中的硫[J].化学分析计量,2018,27(4):28-31.
WANG S,DUAN W Y,CAO C,et al. Determination of sulfur in vehicle diesel oil by tube furnace combustion with ion chromatography[J].Chemical analysis and meterage,2018,27(4):28-31.
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