Abstract:The industrial silicon sample was dissolved with hydrofluoric acid and nitric acid. After removing silicon and fluorine by perchloric acid fuming, ascorbic acid and the color developing solution were added successively for coloring followed by direct determination. Thus, an analysis method of phosphorus content (0.001%-0.27%) in industrial silicon by phosphomolybdenum blue spectrophotometry was established. The results showed that Beer’s law was obeyed for mass concentration of phosphorus in range of 0.05-1.40 μg/ mL. The detection limit of method was 0.000 46 μg/mL. The apparent molar absorptivity was ε825=2.75×104 L·mol-1·cm-1. Other coexisting ions in sample had no interference. The content of phosphorus in three industrial silicon industry reference materials was determined according to the experimental method in different laboratories, and the results were consistent with the certified values. The content of phosphorus in two industrial silicon industry reference materials was determined according to the experimental method, and the results were both consistent with those obtained by national standard methods GB/T 14819.4-2012 and GB/T 14819.5-2012. The proposed method was applied to the determination of phosphorus (0.001%-0.27%) in industry reference materials and actual samples of industrial silicon. The relative standard deviations (RSD, n=22) were between 1.4% and 4.5%.
安中庆,赵德平,方海燕,刘维理,刘英波,周 娅. 磷钼蓝分光光度法测定工业硅中磷[J]. 冶金分析, 2016, 36(12): 74-78.
AN Zhong-qing,ZHAO De-ping,FANG Hai-yan LIU Wei-li,LIU Ying-bo,ZHOU Ya. Determination of phosphate in industrial silicon by phosphomolybdenum blue spectrophotometry. , 2016, 36(12): 74-78.
Tsang S, Phu F, Baum M M,et al. Determination of phosphate/arsenate by a modified molybdenum blue method and reduction of arsenate by S2O42-[J].Talanta,2007,71:1560-1568.
李山,刘丹.磷钼蓝分光光度法测定环境水样中无机磷[J].冶金分析,2006,26(3):82-83.LI Shan,LIU Dan.Spectrophotometric determination of inorganic phosphorus in environmental water samples with phospho molybdenum blue[J].Metallurgical Analysis,2006,26(3):82-83.
[4]
刘少民,谢跃勤.磷钼蓝吸光光度法测定水样中磷[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B: Chemical Analysis),1999,35(1):40.
[5]
Dhavile S M,Shekhar R,Thangavel S, et al. Determination of trace phosphorus in zirconium-niobium alloy and zircaloy by UV-vis spectrophotometry[J].Talanta,2008,76(1):134-137.
朱延宁,景维贤,卢利军,等.磷钼蓝光度法测定金属硅中痕量磷[J].检验检疫科学(Journal of Inspection and Quarantine),1999,9(3):55-56.
[8]
周红.磷钼兰比色法测定工业硅中的磷[J].贵州化工,2002,27(1):21-22.ZHOU Hong.Spectrophotometric determination of phosphorus in metal silicon by phosphomolybdenum blue[J].Guizhou Chemical ldustry,2002,27(1):21-22.
[9]
唐维学,张永进,阮勇防.磷锑钼三元杂多蓝光度法测定工业硅中的磷[J].广东有色金属学报,1999,9(2) :153-155.TANG Wei-xue,ZHANG Yong-jin, RUAN Yong-fang.Determination of phosphorus in silicon metal by P-Sb-Mo ternary heteropoly blue spectrophotometry[J].Journal of Guangdong Non-Ferrous Metals,1999,9(2):153-155.
[10]
李清彩,赵庆令,荀红梅,等.电感耦合等离子体原子发射光谱法测定多金属矿石中砷镉铟硫锑[J].冶金分析,2015,35(2):61-64.LI Qing-cai,ZHAO Qing-ling,XUN Hong-mei,et al.Determination of arsenic,cadmium,indium,sulfur and antimony in polymetallic ore inductively coupled plasma atomic emisson spectrometry [J].Metallurgical Analysis,2015,35(2):61-64.
[11]
李核,田俊,黄艳芳,等.密闭消解磷钼蓝光度法测定多晶硅中磷[J].冶金分析,2011,31(8):61-64.LI He,TIAN Jun,HUANG Yan-fang,et al. Determination of phosphorus in polycrystalline silicon by phosphorus molybenum blue spectrophotometry with closed digestion [J]. Metallurgical Analysis, 2011, 31(8): 61-64.