Abstract：Silicon and phosphorus are the key indexes for the quality of iron ore. Accurate and rapid determination of silicon and phosphorus content is of great significance to determine the economic value of iron ore and establish the smelting process. The iron ore samples were decomposed and dissolved in hydrochloric acid-nitric acid-hydrofluoric acid mixed system by microwave digestion. Then the contents of silicon and phosphorus were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The digestion effects in different systems were tested, and the results showed that the digestion system of hydrochloric acid-nitric acid-hydrofluoric acid mixture had best digestion efficiency. The calibration curve was prepared by matrix matching method in 5% mixed acid as testing medium to eliminate the influence of matrix effect. The linear correlation coefficients of calibration curves for silicon and phosphorus were both higher than 0.999 9. The limit of detection (LOD) was 0.076% and 0.000 94% for silicon and phosphorus, respectively. The contents of silicon and phosphorus in certified reference materials of iron ore such as GSB03-2854-2012 were determined according to the experimental method. The relative standard deviations (RSD, n=6) of determination results were between 0.15% and 1.9%. The found results had no significant difference with the certified values. The iron ore sample NIL PT-1798-2 for proficiency testing was determined according to the experimental method, and the results were satisfactory.
王越, 孙景晓, 王现杰, 辛丽莎, 刘泉秀. 微波消解-电感耦合等离子体原子发射光谱法测定铁矿石中硅和磷[J]. 冶金分析, 2021, 41(2): 44-48.
WANG Yue, SUN Jingxiao, WANG Xianjie, XIN Lisha, LIU Quanxiu. Determination of silicon and phosphorus in iron ore by microwave digestion-inductively coupled plasma atomic emission spectrometry. , 2021, 41(2): 44-48.
王东,刘善军,毛亚纯,等.鞍山式铁矿SiO2含量的热红外光谱分析方法[J].光谱学与光谱分析,2018,38(7):2101-2106.WANG Dong,LIU Shanjun,MAO Yachun,et al. A method based on thermal infrared spectrum for analysis of sio2 content in anshan-type iron[J].Spectroscopy and Spectral Analysis,2018,38(7):2101-2106.
[2]
张庆建,岳春雷,郭兵,等.微波消解-电感耦合等离子体发射光谱测定铜精矿中的银[J].分析科学学报,2017,33(4):582-584.ZHANG Qingjian,YUE Chunlei,GUO Bing,et al.Determination of silver in copper concentrates by microwave digestion and inductively coupled plasma-optical emission spectrometry[J].Journal of Analytical Science,2017,33(4):582-584.
[3]
高小飞,张红丽,毛香菊,等.电感耦合等离子体原子发射光谱法测定钨精矿中钼[J].理化检验(化学分册),2017,53(8):962-964.GAO Xiaofei,ZHANG Hongli,MAO Xiangju,et al.Determination of molybdenum in tungsten concentrate by inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2017,53(8): 962-964.
[4]
秦明,朱尧伟,班俊生,等.微波消解-电感耦合等离子体发射光谱法测定多金属矿中10种主次元素[J].化学分析计量,2019,28(2):45-49.QIN Ming,ZHU Yaowei,BAN Junsheng,et al.Determination of 10 major and minor elements in polymetallic ore by microwave digestion-ICP-AES[J].Chemical Analysis and Meterage,2019,28(2):45-49.
[5]
郑智慷,曾江萍,王家松,等.常压密闭微波消解-电感耦合等离子体发射光谱法测定锑矿石中的锑[J].岩矿测试,2020,39(2):208-215.ZHENG Zhikang,ZENG Jiangping,WANG Jiasong,et al.Determination of antimony in antimony ores by inductively coupled plasma-optical emission spectrometry with microwave digestion[J].Rock and Mineral Analysis,2020,39(2): 208-215.
[6]
冯宗平.电感耦合等离子体原子发射光谱法测定铁矿石中16种元素[J].冶金分析,2019,39(11);57-62.FENG Zongping.Determination of sixteen elements in iron ore by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2019, 39(11): 57-62.
[7]
张为,赵嘉微,王琳.ICP-AES分析高盐样品时雾化器堵塞问题的研究[J].光谱实验室,2004,21(5):977-978.ZHANG Wei,ZHAO Jiawei,WANG Lin,Investigation on blockade of nebulizer in determination of the saline samples by ICP-AES[J].Chinese Journal of Spectroscopy Laboratory,2004,21(5):977-978.
[8]
庞晋山,黄刚,邓爱华,等.电感耦合等离子体原子发射光谱分析中易电离元素的基体干扰及其抑制的研究[J].理化检验(化学分册),2012,48(6):671-677.PANG Jinshan,HUANG Gang,DENG Aihua,et al. Study on the matrix interference of easily ionized elements in ICP-AES and its suppression [J]. Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2012,48(6):671-677.
[9]
武汉大学.分析化学[M].北京:高等教育出版社,2006.
[10]
黄超冠,蒙义舒,郭焕花,等.过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铝合金中的铬铁钼硅[J].岩矿测试,2020,39(2):208-215.HUANG Chaoguan,MENG Yishu,GUO Huanhua,et al.Determination of chromium, iron, molybdenum and silicon in Ti-Al alloy by inductively coupled plasma-optical emission spectrometry with sodium peroxide alkali fusion[J].Rock and Mineral Analysis,2020,39(2):208-215.
[11]
张婉玉,刘喜财.电感耦合等离子体发射光谱法测定锰矿石中铝、钙等多种元素[J].山西化工,2015 (3):41-42,47.ZHANG Wanyu,LIU Xicai.ICP-AES determination of aluminum, calcium and other elements in manganese [J].Shanxi Chemical Industry,2015(3):41-42,47.
[12]
赵希文,朱春要,董礼男,等.电感耦合等离子体原子发射光谱(ICP-AES)法测定铁矿石中钒[J].中国无机分析化学,2020,10(1):62-65.ZHAO Xiwen,ZHU Chunyao,DONG Linan,et al.Determination of vanadium in iron ore by inductively coupled plasma atomic emission spectrometry [J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(1): 62-65.
[13]
王伟,王莹,潘春秀,等. ICP-AES同时测定铁矿石中铅、砷、锌、铜、钾[J].广州化工,2020,48(1):83-85.WANG Wei,WANG Ying,PAN Chunxiu,et al.Determination of Pb, As, Zn, Cu and K in iron ore by inductively coupled plasma-atomic emission spectrometry [J]. Guangzhou Chemical Industry,2020,48(1):83-85.
