摘要
利用闪蒸汽化装置对试样进行气化和计量,采用分光光度法建立了1-丁烯和丁二烯等碳四烯烃中微量羰基化合物的分析方法。对分析条件进行了优化,绘制了校准曲线,并考察了该分析方法的实际运用效果。实验结果表明,优选的分析条件为:两级吸收管串联、气体流量0.3L/min、33%(w)氢氧化钾水溶液和无羰基甲醇按体积比1:2混合、测定波长530.0nm、显色时间23~33min之间。以丁酮为标样得到标准溶液的净吸光度校准曲线,在羰基化合物含量为0~60μg和0~240μg范围内,净吸光度和羰基化合物含量均呈良好的线性关系,线性相关系数大于0.999,回收率在101%-110%之间,重复性良好,羰基化合物含量的最低检测限设定为0.5mg/kg。
A spectrophotometry with a flash evaporator was established to determined trace carbonyl compounds in C4 olefins(1-butene and 1, 3-butadiene). The analyzing conditions were optimized, the standard curves were described and actual samples were analyzed. The results indicated that the optimized conditions were: gas flow rate 0.3 L/min, determining wave length 530 nm, volume ratio of 33%(w) KOH solution to methanol without carbonyl compounds 1 : 2, and coloring time 23-33 min. The standard curves with 2-butanone as the standard sample showed that there were good linear relationships between the content of the trace carbonyl compounds in the content ranges of 0-60 μg and 0-240 μg and the net absorbance of the standard solution, the correlation coefficients were more than 0.999, the recoveries were in the range of 101%-110%, all the relative standard deviations for 5 tests were less than 10%, and the detection limit of carbonyl compounds should be at 0.5 mg/kg.
出处
《石油化工》
CAS
CSCD
北大核心
2015年第10期1256-1261,共6页
Petrochemical Technology