摘要
通过对生物柴油样品进行皂化,建立了一种测定生物柴油中磷含量的方法。红外分析表明生物柴油与KOH反应生成了固态皂,对生成的皂在680℃下进行灰化,再通过钼蓝比色测定样品的磷含量。固态皂的生成克服了液态生物柴油前处理过程中的样品飞溅、燃烧等安全隐患与样品损失,提高了方法的精密度、准确度和效率。皂的灰化产物为易溶性磷酸盐,从而避免了后续的繁琐操作。所建立方法的回收率在96.3%~105.1%之间,RSD均小于2.8%,方法的检测限为0.36 mg/kg,定量限为1.22 mg/kg,对实际样品的检测结果与国标所采纳的ICP-OES法相当。所建立的方法不依赖于大型仪器,成本较低,准确度和精密度较高,可满足生物柴油中磷含量日常检测的需要。
A method for the determination of phosphorus content in biodiesel was established.Soap was formed by saponification reaction through the addition of KOH into biodiesel samples and confirmed by fourier transform infrared spectroscopy(FTIR).The obtained soap was ashed at 680℃and the phosphorus content of the sample was measured by molybdenum blue colorimetry.Compared with the ashing for the liquid biodiesel samples,the ashing technique of solid soap not only alleviated the security concerns such as splashing and burning,but also improved the accuracy,precision and efficiency of the method.Meanwhile,the formation of the soluble potassium phosphate avoided the subsequent cumbersome operations.The recoveries of the method were between 96.3%and 105.1%,and RSDs were less than 2.8%.The detection limit was 0.36 mg/kg and the limit of quantification was 1.22 mg/kg.The phosphorus contents obtained by this method were equivalent to those obtained by ICP-OES method.The present method,which has advantages such as low cost,high accuracy and precision,can be used as an alternative method for the routine analysis of phosphorus content in biodiesel samples without using large-scale instrument.
作者
陈斌
窦泽坤
李蓉
杨赛
马晓迅
黄飞
CHEN Bin;DOU Zekun;LI Rong;YANG Sai;MA Xiaoxun;HUANG Fei(School of Chemical Engineering,Northwest University,Xi′an 710069,China;Guangdong Zhuoyuan New Material Technology Co.LTD,Zhongshan 528458,China)
出处
《西北大学学报（自然科学版）》
CAS
CSCD
北大核心
2018年第2期209-213,共5页
Journal of Northwest University（Natural Science Edition）
基金
国家自然科学基金资助项目(21376191)
陕西省教育厅产业化培植基金资助项目(2013JC23)
陕西省教育厅服务地方专项计划基金资助项目(14JF027)
陕西省自然科学基金资助项目(2011JM2013)
关键词
生物柴油
皂化
钼蓝比色法
磷含量
biodiesel
saponification
Molybdenum blue colorimetry
Phosphorus content
