Determination of iron in low-iron quartz sand by high resolution continuum source graphite furnace atomic absorption spectrometry
ZHANG Liping1,2,3, YAO Mingxing*1,2,3, ZHANG Hongli1,2,3, XIAO Fang1,2,3, NI Wenshan1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. National Engineering Research Center for Comprehensive Utilization of Non-Metallic Mineral Resources, Zhengzhou 450006, China; 3. Key Laboratory for Polymetallic Ore Evaluation and Utilization, MNR, Zhengzhou 450006, China
Abstract:The development of innovative application technology of low-iron quartz resources required the accurate determination of iron content which was the key element affecting its quality. The sample was presoaked in 15 mL of hydrofluoric acid and 2 mL of nitric acid at 150 ℃ for 2 hours. Then 2 mL of perchloric acid was added for open acid digestion at 180 ℃. Finally, the extraction was conducted with 1 mL of nitric acid and 1 mL of water. The content of iron in the sample solution was determined by high resolution continuum source graphite furnace atomic absorption spectrometer at 248.327 nm. A method for determination of trace impurity iron in low-iron quartz sand was established. The experimental conditions including sample dissolution method, temperature program of graphite furnace, atomization reading time and effective pixels were optimized. The results showed that when the mass concentration of iron was in range of 20-100 ng/mL, the determination coefficient of the calibration curve equation between absorbance and mass fraction fitted by the least square method was up to 0.999 8. The limit of detection of method was 0.002 49 μg/g, and the limit of quantification was 0.007 47 μg/g. The content of impurity iron in eight low-iron quartz samples was determined according to the experimental method. The results were basically consistent with those obtained by inductively coupled plasma mass spectrometry. The relative standard deviation (RSD, n=5) of determination results were between 2.2% and 4.8%. The standard solution of iron was added for recovery tests. The recoveries were between 90% and 110%, which could meet the requirements of recovery in the national geological and mineral industry standard of DZ/T0130-2006.
[1] 汪灵,李彩侠,王艳,等.高纯石英质量的ICP检测技术研究与应用[J].光谱学与光谱分析,2013(6):1684-1688. WANG Ling,LI Caixia,WANG Yan,et al.Research on and application of the ICP detection technology for the quality of high-purity quartz[J].Spectroscopy and Spectral Analysis,2013(6):1684-1688. [2] 贾德龙,张万益,陈丛林,等.高纯石英全球资源现状与我国发展建议[J].矿产保护与利用,2019,39(5):111-117. JIA Delong,ZHANG Wanyi,CHEN Conglin,et al.Global resource status and China's development suggestions of high purity quartz[J].Protection and Utilization of Mineral Resources,2019,39(5):111-117. [3] 汪灵.石英的矿床工业类型与应用特点[J].矿产保护与利用,2019,39(6):39-47. WANG Ling.Industrial type and application characteristics of quartz ore deposits[J].Protection and Utilization of Mineral Resources,2019,39(6):39-47. [4] 苏梦晓,陆安军.电感耦合等离子体原子发射光谱-内标法测定优质石英砂中8种杂质组分[J].冶金分析,2020,40(4):36-43. SU Mengxiao,LU Anjun.Determination of eight impurities in high quality quartz sand by inductively coupled plasma atomic emission spectrometry-internal standard method[J].Metallurgical Analysis,2020,40(4):36-43. [5] 孔芹,陈磊,汪灵.非金属矿二级标样配制及其粉末样品的XRF分析方法[J].光谱学与光谱分析,2012,32(5):1405-1409. KONG Qin,CHEN Lei,WANG Ling.Preparation of sub-standard samples and XRF analytical method of powder non-metallic minerals[J].Spectroscopy and Spectral Analysis,2012,32(5):1405-1409. [6] 杭义萍,谢增春,吴彩云.ICP-AES同时测定高纯石英砂中硼和磷含量[J].光谱实验室,2010,27(4):1503-1506. HANG Yiping,XIE Zengchun,WU Caiyun.Simultaneous determination of boron and phosphorus in purifying high grade quartz sand by ICP-AES[J].Chinese Journal of Spectroscopy Laboratory,2010,27(4):1503-1506. [7] 李茂巨,王基伟,孙继南.溶剂萃取原子吸收光谱法测定高纯石英砂中痕量铁[J].山东国土资源,2005,21(10):53-55. LI Maoju,WANG Jiwei,SUN Jinan,et al.Determining trace iron element in pure quartz by using extraction-atomic absorption spectrophotometry[J].Land and Resources of Shandong,2005,21(10):53-55. [8] 林益,薛理辉,铁丽云.高纯石英砂中微量铁的测定[J].中国非金属矿工业导刊,1998(4):34-35. LIN Yi,XUE Lihui,TIE Liyun.The determination of trace Fe in high purity quartz sand[J].China Non-metallic Minerals Industry Guide,1998(4):34-35. [9] 张宏丽,倪文山,刘磊,等.冷焰模式-电感耦合等离子体质谱法测定高纯石英中痕量铁[J].冶金分析,2021,41(7):28-34 ZHANG Hongli,NI Wenshan,LIU Lei,et al.Determination of trace iron in high-purity quartz by cool flame mode-inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2021,41(7):28-34. [10] 陈京京,陈静,卞卫东.火焰、石墨炉原子吸收法测定自来水中微量铁[J].中国资源综合利用,2011,29(12):35-37. CHEN Jingjing,CHEN Jing,BIAN Weidong.To detect trace iron in tap water with FAAS and EAAS[J]. China Resources Comprehensive Utilization,2011,29(12):35-37. [11] 刘焕敏,吴洁,王京侠,等.石墨炉原子吸收光谱法测定石英玻璃中痕量铁检出限的探讨[J].中国建材科技,2021,30(1):27-29. LIU Huanmin,WU Jie,WANG Jingxia,et al.Determination of trace iron detection limit in quartz glass by graphite furnace atomic absorption spectrometry[J].China Building Materials Science & Technology,2021,30(1):27-29. [12] 汪雨,陈舜琮,杨啸涛.连续光源原子吸收光谱法的研究进展及应用[J].冶金分析,2011,31(2):38-47. WANG Yu,CHEN Shuncong,YANG Xiaotao.Research progress and application of continuum source atomic absorption spectrometry[J].Metallurgical Analysis,2011,31(2):38-47. [13] 高燕,刘英.石墨炉原子吸收法测定高纯硒中痕量铁[J].分析试验室,2007(3):26-29. GAO Yan,LIU Ying.Determination of trace iron in high-purity selenium by GFAAS[J].Chinese Journal of Analysis Laboratory,2007(3):26-29. [14] 卢桂萍,汪正,邱德仁,等.悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、铁和钠含量[J].光谱学与光谱分析,2011,31(1):244-248. LU Guiping,WANG Zheng,QIU Deren,et al.Direct determination of copper, iron and sodium in high-purity alumina by slurry introduction furnace atomic absorption spectrometry with Smith-Hieftje background correction[J].Spectroscopy and Spectral Analysis,2011,31(1):244-248. [15] 中华人民共和国国土资源部.DZ/T 0130—2006地质矿产实验室测试质量管理规范[S].北京:中国标准出版社,2006.