碱熔电感耦合等离子体原子发射光谱测定润滑脂中的硼  

Determination of Boron in Greases by ICP-AES with Alkali Fusion

作　　者：崔亮[1] 张大华[1] 李进[1] 魏斌斌[1] 王婧[1] Cui Liang;Zhang Dahua;Li Jin;Wei Binbin;Wang Jing(Lanzhou Lubricating Oil R&D Institute,PetroChina,Lanzhou 730060,China)

机构地区：[1]中国石油兰州润滑油研究开发中心,兰州730060

出　　处：《合成润滑材料》2020年第4期7-10,共4页Synthetic Lubricants

摘　　要：现有的测定硼含量的方法(SH/T0749方法,GB/T17476和NB/SH/T0824方法)均只适合测定润滑油及添加剂中的硼,不适用于测定润滑脂中的硼,为此建立了一种用电感耦合等离子体发射光谱测定润滑脂中硼含量的方法。用氢氧化钾对润滑脂样品进行碱熔灰化预处理,氢氧化钾的用量约2.0 g,并用5.0 mL浓盐酸中和,灰化温度为550℃,灰化时间为15.0 min。等离子体发射光谱的冷却气流量为14.5 L/min,辅助气流量为1.4 L/min,雾化器流量为0.70 L/min,射频功率为1400 W。回归分析的相关系数达到了0.9999,加标回收率在94%~105%之间,相对标准偏差不超过3.0%,说明建立的测定润滑脂中硼含量方法的准确性好,精密度高,能够满足润滑脂中的硼元素含量的测定要求。The existing methods(SH/T07449,GB/T17476 and NB/SH/T0824)for determining boron content were only suitable for the determination of boron in lubricating oils and additives,but not in grease.So a method for the determination of boron content in grease was established by ICP-AES.The grease samples were pretreated by alkali fusion ashing with potassium hydroxide.The dosage of potassium hydroxide was about 2.0 g and neutralized with 5.0 mL concentrated hydrochloric acid.The ashing temperature was 550℃and the ashing time was 15.0 min.Its cooling gas flow rate,auxiliary gas,atomizer and radio frequency(RF)power were 14.5 L/min,1.4 L/min,0.70 L/min and 1400 W respectively.The correlation coefficient of regression analysis was 0.9999,the recovery was between 94%and 105%,and the relative standard deviation was less than 3.0%.The results showed that the established method had good accuracy and high precision,and could meet the requirements of determination of boron content in lubricating greases.

关 键 词：灰化温度 灰化时间 工作参数 

分 类 号：TE626.4[石油与天然气工程—油气加工工程]