Separation and determination of sulfur and samarium in samarium sulfide
ZHANG Hong1,2,3, REN Xu-dong1,2, HAO Qian1,2
1.Baotou Research Institute of Rare Earth, Baotou 014030, China; 3. School of Chemistry and Biological Engineering,University of Science and Technology Beijing,Beijing 100083, China
Abstract：A simultaneous determination method of sulfur and samarium in samarium sulfide was studied. The samarium sulfide sample was fused with sodium hydroxide and sodium peroxide. The S2- was totally oxidized to S6+. After separation twice with ammonia water, the filtrate at pH 2-5 was heated to boiling. The barium chloride solution was added to precipitate the sulfate. Then, the content of sulfur could be calculated. The samarium hydroxide precipitate was acidified with hydrochloric acid followed by titration with EDTA standard solution. Then, the content of samarium could be determined. The conditions were obtained by orthogonal experiments: fusion at 550 ℃ for 10 min;the aging was not required during the precipitation of sulfate using barium chloride solution. The variance analysis indicated that the ammonia water separation times and precipitation pH values were significant factors influencing the experimental results. The optimal separation times by ammonia water was twice, and the pH for precipitation was 2-5. In addition, the results proved that the experimental results were not affected by the nickel introduced in sample fusion from nickel crucible. The precision of samarium sulfide sample was investigated according to the experimental method. The relative standard deviation (RSD) for sulfur and samarium was 0.73% and 0.18%, respectively. The recovery test of standard addition indicated that the recoveries for sulfur and samarium were 101%-103% and 100%-102%, respectively. Two samarium sulfide samples were determined according to the experimental method, and then compared with the determination results of sulfur by barium chloride titration and samarium by oxalate gravimetry. The found results were in good agreement. Compared to the single element determination method, the repeated sample fusion was avoided in proposed method, reducing the pretreatment process of sample. The simultaneous determination of sulfur and samarium was realized. The proposed method could be used in routine production and analysis.
黄剑锋,曹丽云.双靶溅射法制备M-SmS光学薄膜的研究[J].材料科学与工艺,2004,12(1):1-3.HUANG Jian-feng,CAO Li-yun.The forming of M-SmS optical thin films deposited by co-sputtering[J].Materials Science and Technology,2004,12(1):1-3.
[2]
Hickey C F.Optical, chemical and structural properties of thin films of samarium-sulfide and zinc-sulfide[D]Tucson: University of Arizona,1987.
[3]
张翼眀,任旭东,郝茜,等.惰气熔融-红外吸收法测定硫化钐中氧的不确定度评价[J].稀土,2014,35(4):88-91.ZHANG Yi-ming,REN Xu-dong,HAO Qian,et al.Evaluation on the uncertainty for determining oxygen in SmS by inert gas fusion-infrared absorption method[J].Chinese Rare Earths,2014,35(4):88-91.
庄艾春,肖红新.红外碳硫仪测定矿石中高含量硫的探讨[J].岩矿测试,2009,28(1):79-80.ZHUANG Ai-chun,XIAO Hong-xin.Determination of high-content sulfur in ores by infrared carbon-sulfur analyzer[J].Rock and Mineral Analysis,2009,28(1):79-80.
[6]
肖红新.红外吸收法测定铅锌矿中的高硫[J].广东有色金属学报,2005,15(1):70-72.XIAO Hong-xin.Determination of high sulfur in lead-zinc mine with infrared absorption method[J].Journal of Guangdong Non-Ferrous Metals,2005,15(1):70-72.
[7]
郑大中,李小英,郑若锋,等.过氧化钠超强熔矿能力的新认识[J].四川地质学报,2010,30(4):488-499.ZHENG Da-zhong,LI Xiao-ying,ZHENG Ruo-feng,et al.The application of coherency cube and image sharpening to seismic data interpretation[J].Acta Geologica Sichuan,2010,30(4):488-499.
[8]
姜大伟,于伟江.水泥中三氧化硫含量测定方法的操作要点[J].辽宁建材(LiaoNing Building Materials),2011,32(12):36-37.
[9]
王雪莹,陈怀燕,王冰莹.硫酸钡重量法测定硫精矿与硫铁矿中全硫[J].冶金分析,2010,30(增):758-760.WANG Xue-ying,CHEN Huai-yan,WANG Bing-ying.Determination of total sulfur content in pyrites and concentrate by barium sulphate gravimetric method[J].Metallurgical Analysis,2010,30(Suppl.):758-760.
[10]
王瑞斌.高岭土中全硫量快速测定方法[J].岩矿测试,2006,25(1):82-84.WANG Rui-bin.Rapid method for the determination of total sulphur content in Kaolin[J].Rock and Mineral Analysis,2006,25(1):82-84.
[11]
董亦斌.玫瑰红钠试纸作外指示剂-氯化钡滴定法测定水中硫酸根[J].冶金分析,2013,33(4):61-63.DONG Yi-bin.Determination of sulfate radical in water by barium chloride titration with sodium rhodizonate test paper as external indicator[J].Metallurgical Analysis, 2013,33(4):61-63.
