摘要
对WK-2D型微库仑仪进行调试.从进样量、进样速度、气体流量、炉温4个方面讨论操作因素对微库伦法测定样品硫含量的影响,并确定最优操作条件.在优化条件下,对加标直馏柴油样品进行精密度和回收率考察.结果表明：进样量为1.3μL,进样速度为38档,氮气流量为260 mL/min,氧气流量为150 mL/min,汽化段温度为750℃,燃烧段温度为850℃,稳定段温度为650℃操作条件下测得直馏柴油硫含量误差低,重复性好.加标回收率在99％～102％,RSD＜1％.该方法简单、快速、准确,适合大批量直馏柴油样品的测定.
The WK-2D microcoulometer was tuned.The injection volume,injection rate,gas flow rate,furnace temperature,four aspects which impact on the determination of sulfur content of the sample by micro-coulometry were discussed.and the appropriate formula and technologic condition were determined.Under optimization conditions,the precision and recovery rate of straight-run diesel spiked were studied.The results indicated：the injection volume was 1.3μL,injection speed of 38 scale.nitrogen flow 260 mL/min,the oxygen flow 150 mL/min,the vaporization segment temperature of 750 ℃,the combustion segment temperature of 850 ℃,the stable segment temperature of 650 ℃.The method of determination of sulfur content in straight-run diesel oil was reproducible,low error.The recovery was around 99 ％～102 ％ and their RSD values were all lower than 1％.The method was simple,rapidness,accurate and fully suitable for large quantities of determination in the sulfur content of straightrun diesel oil.
出处
《化工科技》
CAS
2013年第4期39-42,共4页
Science & Technology in Chemical Industry
关键词
微库伦法
ρ(硫)
进样量
进样速度
气体流量
炉温
Micro-coulometry
Sulfur content
Injection volume
Injection rate
Gas flow rate
Furnace temperature
