Determination of bromine in carnallite by kinetic energy discrimination in collision cell-inductively coupled plasma mass spectrometry
ZHANG Hong-li1, 2, 3, GAO Xiao-fei1, 2, 3, YAO Ming-xing1, 2, 3, NI Wen-shan*1, 2, 3, SUN Qi-liang1, 2, 3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Northwest China Center for Geoscience Innovation, Xi′an 710054, China
Abstract：Bromine in carnallite sample was dissolved by hot water leaching. The interference of multi-atomic molecular ions was eliminated using kinetic energy discrimination (KED) in collision cell as the measurement mode. 50.0ng/mL 187Re was selected as the internal standard for correction. Consequently the determination method of bromine in carnallite by inductively coupled plasma mass spectrometry (ICP-MS) was established. The hot water leaching time and the flow rate of helium gas were optimized and the following conditions were used: the leaching time was 10min and the flow rate of helium was 4.7mL/min. The matrix effect was investigated and the results showed that it could be effectively overcome by controlling the mass concentration of the solution to be no more than 0.50mg/mL. The standard solution series of bromine were determined under the optimized experimental conditions. The results indicated that the mass concentration of bromine in range of 0.100-400ng/mL was linear to the mass spectrometry intensity with correlation coefficient of 0.9996. The detection limit was 0.424μg/g and the low limit of determination was 1.41μg/g. The proposed method was applied for the determination of bromine in five carnallite samples with different bromine contents. The relative standard deviations (RSD, n=9) were between 1.7% and 4.7%. The spiked recovery test and method comparison test were also conducted. The spiked recoveries were between 98% and 108%. The found results were basically consistent with those obtained by the magenta spectrophotometry.
张宏丽, 高小飞, 姚明星, 倪文山, 孙启亮. 动能歧视碰撞池-电感耦合等离子体质谱法测定光卤石中溴[J]. 冶金分析, 2019, 39(8): 14-18.
ZHANG Hong-li, GAO Xiao-fei, YAO Ming-xing, NI Wen-shan, SUN Qi-liang. Determination of bromine in carnallite by kinetic energy discrimination in collision cell-inductively coupled plasma mass spectrometry. , 2019, 39(8): 14-18.
靳芳,王洪彬,王英.电感耦合等离子体原子发射光谱法测定光卤石矿中钾、钠、钙、镁和硫酸根[J].理化检验:化学分册,2011,47(10):1198-1199.JIN Fang,WANG Hong-bin,WANG Ying.ICP-AES determination of potassium,sodium,calcium,magnesium and sulfate in carnallite[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2011,47(10):1198-1199.
[2]
张力军,王薇,王修林.溴素生产技术及溴系列产品的开发[J].海洋科学,1998(5):20-22.ZHANG Li-jun,WANG Wei,WANG Xiu-lin.Introduction to technique of manufactruing bromineand prospecting development trend in bromined products[J].Marine Science,1998(5):20-22.
[3]
岩石矿物分析编写组.岩石矿物分析[M].3版.北京:地质出版社,1991:219-231.
[4]
王旭日,贾振亚,陈盛,等.电感耦合等离子体质谱法测定水体中溴和碘量[J].理化检验:化学分册,2015,51(8):1187-1190.WANG Xu-ri,JIA Zhen-ya,CHEN Sheng,et al.ICP-MS determination of bromine and iodine in waters[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(8):1187-1190.
[5]
秦愫妮,雷超海,俞建国,等.电感耦合等离子体质谱法同时测定地表水中的溴和碘[J].中国卫生检验杂志,2018,28(15):1814-1820.QIN Su-ni,LEI Chao-hai,YU Jian-guo,et al.Determination of bromide and iodine in surface water by inductively coupled plasma mass spectrometry[J].Chinese Journal of Health Laboratory Technology,2018,28(15):1814-1820.
[6]
杨林,于珊.碰撞反应电感耦合等离子体质谱法直接测定卤水中的溴碘[J].岩矿测试,2013,32(3):502-505.YANG Lin,YU Shan.Direct measurement of Br and I in brines by collision response-inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2013,32(3):502-505.
[7]
Xu L,Luo C,Ling H,et al.Determination of low bromine (Br) and iodine (I) in water with low- to high-salinity content using ICP-MS[J].International Journal of Mass Spectrometry,2018,432:52-58.
[8]
王斌,刘巍瓶,王荣,等.离子色谱法测定钾盐矿种硫酸根和溴离子的含量[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2018,54:806-809.
[9]
袁红战,武丽平,杨林.电感耦合等离子体-质谱法测定固体盐中的溴和碘[J].化学工程师,2018,32(7):39-41.YUAN Hong-zhan,WU Li-ping,YANG Lin.Determination of Br and I in solid salt by inductively coupled plasma-mass spectrometry[J].Chemical Engineer,2018,32(7):39-41.
[10]
张旭,李文波,马成冰,等.X射线荧光光谱法测定光卤石中成分[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2017,53(7):818-820.
[11]
任凤莲,黎艳平.流动注射原子吸收法测定光卤石中钙和镁[J].矿冶工程,1996,16(3):56-59.REN Feng-lian,LI Yan-ping.Determination of Ca2+ and Mg2+ in carnallite by flow injection-atomic absorption spectroscopy[J].Mining and Metallurgical Engineering,1996,16(3):56-59.
[12]
刘环,康佳红,王玉学.碱熔-电感耦合等离子体质谱法测定地质样品中铍铯镓铊铌钽锆铪铀钍[J].冶金分析,2019,39(3):26-32.LIU Huan,KANG Jia-hong,WANG Yu-xue.Determination of beryllium, cesium,gallium,thallium,niobium,tantalum,zirconium,hafnium,uranium and thorium in geological sample by inductively coupled plasma mass spectrometry with alkali fusion[J].Metallurgical Analysis,2019,39(3):26-32.
