摘要
为了简便、准确、快速地测定膨胀石墨中的硫含量,建立了用艾氏卡试剂消化样品、硫酸钡比浊法测定硫含量的方法.实验确定艾氏卡试剂与膨胀石墨最佳物质的量比为1:15,焙烧温度为850℃;比浊法中测试液的pH=1.0,质量分数为5%的聚乙烯醇分散剂和无水乙醇助稳定剂的用量分别为2.0mL和3.0mL;稳定10min后,在460nm下和0.1~5.0mg内,硫酸钡的吸光度符合朗伯-比尔定律;方法平均回收率分别为101.2%(ZnS)和99.5%(Na2SO4),相对标准偏差均不超过3.0%.方法操作简便、准确,能快速测定膨胀石墨中的硫含量.
In order to detect the content of sulfur in expanded graphite(EG), a simple, rapid and accurate method has been proposed. EG samples were digested by Eschka reagent at 850 ℃ with the amount of substance of 15:1 to EG. The absorption of the BaSO4 emulsion was detected at the wavelength of 460 nm after static storage for 10 min. The pH of the detected emulsion was 1.0. A 2.0 mL of 5 % polyvinyl alcohol solution and 3.0 mL ethanol was added as stabile reagent to ensure the formation of steady soliquid. BaSO4 in the range of 0-5.0 mg should be controlled by Lambert-Beer Law. With the RSD not more than 3.0 % , the average recovery is 101.2 % for ZnS and 99.5 % for Na2SO4, respectively. The method is easy and fast to manage and reliable for sulfur measurement in the EG samples.
出处
《河北大学学报(自然科学版)》
CAS
北大核心
2008年第1期52-56,112,共6页
Journal of Hebei University(Natural Science Edition)
基金
河北省教育厅及校内博士基金资助项目(B2004402)
关键词
膨胀石墨
比浊法
艾氏卡试剂
硫转化率
expanded graphite (EG)
turbidimetry
Eschka reagent
percent conversion of sulfur