Extraction and separation of phosphorus by tributyl phosphate for determination of iron, zinc, silicon and aluminum in high purity yellow phosphorus by inductively coupled plasma atomic emission spectrometry
LI Jia1, HUANG Yong-qing2
1. Jiangxi Province Safety Production Science and Technology Research Center Safety Scientific Research Standards, Jiangxi Province Industrial Safety Engineering Technology Research Center, Nanchang 330030,China; 2. Jiangxi Chemical Industry Design Institute of Technology Design Institute,Nanchang 330030,China
Abstract:2g of yellow phosphorus was digested in nitric acid by reflux condensation. The phosphoric acid in high-purity yellow phosphorus digestion solution was extracted and separated using tributyl phosphate (TBP) to reduce the complexation with iron, zinc, silicon and aluminum. Meanwhile, the viscosity of digestion solution for testing could be decreased. The content of iron, zinc, silicon and aluminum was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently the determination method of iron, zinc, silicon and aluminum in high-purity yellow phosphorus by ICP-AES after extraction and separation with TBP was established. The extraction conditions of this method were obtained as below: the volume ratio of sample solution and TBP was 1∶1; the oscillation time was 1min; the standing time was 30min. The mass concentration of elements in range of 0.50-50μg/mL was linear to the corresponding emission intensity. The correlation coefficients (r) of calibration curves were higher than 0.9995. The detection limits of elements were lower than 0.093μg/g. The proposed method was applied for the determination of iron, zinc, silicon and aluminum in yellow phosphorus samples, and the found results were consistent with those obtained by flame atomic absorption spectrometry (FAAS). The relative standard deviations (RSD, n=5) were all less than 0.80%.
李佳, 黄永庆. 磷酸三丁酯萃取分离磷-电感耦合等离子体原子发射光谱法测定高纯黄磷中铁锌硅铝[J]. 冶金分析, 2017, 37(11): 52-58.
LI Jia, HUANG Yong-qing. Extraction and separation of phosphorus by tributyl phosphate for determination of iron, zinc, silicon and aluminum in high purity yellow phosphorus by inductively coupled plasma atomic emission spectrometry. , 2017, 37(11): 52-58.
何家鸿.工业黄磷中磷及微量杂质含量的测定[J].无机盐工业,2008,40(4):57-59.HE Jia-hong.Determination of the contents of phosphorus and trace impurities in the industrial yellow phosphorus[J]. Inorganic Chemicals Industry,2008,40(4):57-59.
[2]
李佳,朱晓帆,许凤兰.磷酸三丁酯萃取-火焰原子吸收光谱法测定高纯黄磷中痕量铁和锌[J].冶金分析,2010,30(10TU):43-46.LI Jia,ZHU Xiao-fan,XU Feng-lan.Determination of trace iron and zinr in high purity yellow phosphorus by flame atomic absorption spectrometry with tributyl phosphate extraction[J]. Metallurigical Analysis,2010,30(10):43-46.
[3]
李佳,朱晓帆,梁进,等.测定黄磷中砷方法的样品前处理的改进[J].理化检验:化学分册,2011, 47(1):92-95.LI Jia,ZHU Xiao-fan,LIANG Jin,et al. Modification for pretreatment of sample in the determination of arsenicin yellow phosphorus[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2011,47(1):92-95.
[4]
杨森泉.Ag-DDTC法测定黄磷中砷含量的研究[J].贵州工业大学学报:自然科学版,2006,35(5):8-11.YANG Sen-quan.Research on the Ag-DDTC determination method for arsenic content in yellow phosphorus[J]. Journal of Guizhou University of Technology:Natural Science Edition,2006,35(5):8-11.
[5]
任永胜,马红琼,李军,等.氢化物发生-原子荧光光谱法测定黄磷中微量砷[J].理化检验:化学分册,2007, 43(7):564-566.REN Yong-sheng,MA Hong-qiong,LI Jun,et al.HG-AFS determination of micro-amounts of arsenic in yellow phosphorus[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2007,43(7):564-566.
[6]
方金东,曹显文.ICP-AES法直接测定黄磷中微量砷[J].冶金分析,1997,17(1):54-55.FANG Jin-dong,CAO Xian-wen. Direct determination of trace arsenic in yellow phosphorus by ICP-AES[J].Metallurigical Analysis,1997,17(1):54-55.
[7]
王光灿,彭莉,朱光辉.电感耦合等离子体发射光谱法测定高纯磷中微量砷[J].云南化工,1998 (2):48-49.WANG Guang-can,PENG Li,ZHU Guang-hui.ICP-AES determination of trace arsenic in purity phosphorus[J].Yunnan Chemical Technology,1998(2):48-49.
[8]
龙光花,梅毅,杨加强,等.电感耦合等离子体原子发射光谱法测定湿法磷酸中8种元素[J].冶金分析,2017,37(6):55-60.LONG Guang-hua,MEI Yi,YANG Jia-qiang,et al.Determination of eight elements in wet-process phosphoric acid by inductiely coupled plasmz atomic emission spectrometry[J]. Metallurigical Analysis, 2017,37(6):55-60.
[9]
许光,邓全道,罗虎,等.电感耦合等离子体发射光谱法同时测定电子级磷酸中14种杂质元素[J].化工技术与开发,2011,40(5):42-45.XU Guang,DENG Quan-dao,LUO Hu,et al.Determination of 14 elements in electronic phosphoric acid by inductively coupled plasma-atomic emissions spectrometric[J].Technology & Development of Chemical Industry,2011,40(5):42-45.
[10]
孙丽丽.电感耦合等离子体发射光谱法湿法精制磷酸中镁、钙、铁、砷含量[J].中国无机分析化学,2013,3(1):71-73.SUN Li-li.Quantitative determination of Mg,Ca,Fe and As in the wet refining process for manufacturing phosphoric acid by ICP-OES[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(1):71-73.
[11]
杨焕银.湿法磷酸溶剂萃取法工艺的研究[J].化肥工业,2001,28(4):15-17.YANG Huan-yin.Study of technology for solvent extraction of wet-process phosphoric acid[J]. Chemical Fertilizer Industry,2001,28(4):15-17.
[11]
刘楠,汪鹏,孟春燕,等.应用电感耦合等离子体质谱法测定污灌白菜中的10种元素[J].环境与职业医学,2016,33(4):398-402.LIU Nan,WANG Peng,MENG Chun-yan, et al.Determination of 10 elements in sewage irrigated cabbage by inductively coupled plasma mass spectrometry[J]. J Environ Occup Med,2016,33(4):398-402.
[12]
欧阳贻德,陈古圣,苏裕光.磷酸三丁酯萃取分离磷酸与盐酸的研究[J].武汉工程大学学报,1998(1):5-9.OUYANG Yi-de,CHEN Gu-sheng,SU Yu-guang.Study of extration and separation of hydrochloric and phosphoric acids by tributyl phosphate[J].Journal of Wuhan Institute of Chemical Technology, 1998(1):5-9.
[13]
李丽华,张金生,陈雨艳.微波消解-火焰原子吸收光谱法测定玉米面中的铜、锌和铁[J].分析科学学报,2009,25(3):337-340.LI Li-hua,ZHANG Jin-sheng,CHEN Yu-yan.Dtermination of Cu,Zn and Fe in maize flour with microwave digestion-flame atomic absorption spectroscopy[J].Journal of Analytical Science,2009,25(3):337-340.
[14]
李志辉,吴玉春,刘海龙.火焰原子吸收光谱法测定铝及铝合金中镉[J].有色矿冶,2001,17(2):45-47.LI Zhi-hui,WU Yu-chun,LIU Hai-long.FAAS determination of cadmium in aluminum and aluminium alloys[J].Non-Ferrous Mining and Metallurgy, 2001,17(2):45-47.