DOI /j. cnki /td ICP - MS 11 MPT ng /L 86. 3% ~ % P641 O O657.

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1 September 2015 ROCK AND MINERAL ANALYSIS Vol. 34 No ~ DOI /j. cnki /td * ICP - MS MPT ng /L RSD 1. 2% ~ 9. 8% 86. 3% ~ % P641 O O A MIP MPT - AES ICP - OES MPT - AES 17 Na X MPT ICP - OES 9-10 MPT ICP - MS MPT MPT ICP Mg Ca Li Cs MPT YQ KJLD yang0905@ 163. com chw8868@ gmail. com 586

2 WGY Ca 2 + MPT - LTQ - XL ThermoFisher Xcalibur 2 a m /z138 m /z156 LTQ Orbitrap XL MPT Ar Thermo Scientific N 2 O 2 NO m /z 50 ~ m /z156 Ca 2 + NO Ca NO 3 2H 2 O + Ca NO 3 3H 2 O m /z138 2 b c m /z120 Ca NO 3 H 2 O + m /z102 Ca NO m /z102 Ca μg /L Ca 2 + m /z156 6 m /z % m /z138 Ca 2 + Ca LTQ Orbitrap MΩ cmxl CaH 4 O 5 N ppm m /z Ca NO 3 2H 2 O + 1 MPT - MS Ca 2 + Fig. 1 Schematic illustration of Microwave plasma torch-mass spectrometer to detect Ca 2 + in water 587

3 http www. ykcs. ac. cn MPT - MS Ca 2 + a b m /z138 c m /z138 Fig. 2 Spectra of Ca 2 + in water samples detected by MPT-MS. a full mass spectrum b MS 2 spectrum of m /z138 c MS 3 spectrum of m /z138 Ca NO 3 H 2 O + 4 a 600 ml /min Ca NO 3 H 2 O + Ca NO 3 H 2 O + 4 b μg /L 5 Ca ~ 1000 μg /L Ca MPT Ca 2 + m /z CaH 4 O 5 N m /z Fig. 3 A comparison of MPT orbitrap mass spectrum of m /z in water samples and standard mass spectrum of CaH 4 O 5 N m /z μg /L Ca 2 + Ca NO 3 H 2 O + 50 W Ca NO 3 H 2 O + 24 Ca NO 3 H 2 O + 4 a b Ca NO 3 Fig. 4 Optimization of parameter. a flow rate of the carrier H 2 O + gas b flow rate of the support gas 588

4 - 34 y = 4. 69x Ca NO 3 H 2 O σ n = 11 S /N = 3 Ca 2 + Ca 2 + LOD = 3σC /S 26 C 1 σ S 86. 3% ~ % ng /L 2. 4 Ca Ca Tabel 1 Analytical results of Ca 2 + in actual samples μg /L μg /L μg /L mg /L R 2 % y = x ~ 30 y = x y = x y = x ~ 100 y = x ~ 75 y = x Purification Technology MPT Xue Y Y Wang X Y He B P et al. The Determination ng /L Research Progress of the Metal Trace Element Iron RSD 1. 2% ~ 9. 8% 86. 3% ~ Copper Zinc Magnesium Calcium by Spectrophotometry % J. Studies of Trace Elements and Health MPT J MPT Chen Z X X B Zheng Y S et al. Determination of Water-soluble Ca and Mg in Soils by High-resolution Continuum Source Atomic Absorption Spectrometry J. Rock and Mineral Analysis Das M Raut V Deb S et al. Determination of Calcium and Iron in Silicon and Uranium Silicide Using Ion Chromatography J. Journal of Radioanalytical and Nuclear Chemistry J. Rock and Mineral Analysis J Su Y L Fang L. Application of Ion-Chromatography Technique in Drinking Water Analysis J. Water 3. J. 5. J Wang Y. High-resolution Continuum Source Atomic Absorption Spectrometer and Its Application in Determination of Metal Ions in Drinking Mineral Water 6 Sowmya R Indumathi K Arora S et al. Detection of Calcium Based Neutralizers in Milk and Milk Products by AAS J. Journal of Food Science and Technology 589

5 http www. ykcs. ac. cn Vahdati-Mashhadian N Balali-Mood M Sadeghi M et al. Determination of Calcium in Mashhad City Tap Water by Flame Atomic Absorption Spectrometry J. Journal of The Chemical Society of Pakistan X Emission Spectroscopy MPT-AES J. Spectroscopy J. and Spectral Analysis Fan X T Zhan X C Gong A H. Determination of Major Elements in Brine Samples by Polarized Radiation- Energy Dispersive X-ray Fluorescence Spectrometry J. Rock and Mineral Analysis Besson P Degboe J Berge B et al. Ca Na K and Mg Concentrations in Seawater by Inductively Coupled Plasma-Atomic Emission Spectrometry Applications to IAPSO Seawater Reference Material Hydrothermal Fluids and Synthetic Seawater Solutions J. Geostandards and Geoanalytical Research Asfaw A Wibetoe G. Simultaneous Determination of Hydride Se and Non-hydride-forming Ca Mg K P S and Zn Elements in Various Beverages Beer Coffee and Milk with Minimum Sample Preparation by ICP-AES and Use of a Dual-mode Sample-introduction System J. Analytical and Bioanalytical Chemistry Yu L L Davis W C Ordonez Y N et al. Fast and Accurate Determination of K Ca and Mg in Human Serum by Sector Field ICP-MS J. Analytical and Bioanalytical Chemistry Feng G D Huan Y F Cao Y B et al. Development of a Miniature Simultaneous MPT Spectrometer J. Microchemical Journal J J Li X X. Determination of Si Mg Ca Sr and K in Mineral Water by Microwave Plasma Torch-Atomic Emission Spestrometry J. Analytical Instrumentation Jia Q Kong X F Zhou W H et al. Flow Injection On-line Preconcentration with an Ion-exchange Resin Coupled with Microwave Plasma Torch-Atomic Emission Spectrometry for the Determination of Trace Rare Earth Elements J. Microchemical Journal Zhang J S Li L H Jin Q H. Determination of Silicon Iron and Vanadium in Petroleum Coke by Microwave Digestion-Microwave Plasma Torch Atomic Emission Spectrometry J. Petroleum Science and Technology J Liang P H Li A M. Determination of Phosphorus and Manganese in Tea by Microwave Plasma Torch Atomic Na Mg Ca Li Cs J Zhou W Xiong H L Feng G D et al. Determination of Sodium Magnesium Calcium Lithium and Strontium in Natural Mineral Drinking Water by Microwave Plasma Torch Spectrometry with Nebulization Sample Introduction System J. Spectroscopy and Spectral Analysis J Zhang T Q Jin W Zhou J G et al. Rapid Detection of Active Pharmaceutical Ingredients in Drugs by Microwave Plasma Atmospheric Pressure Desorption Ionization Mass Spectrometry J. Chemical Journal of Chinese Universities Zhang T Q Zhou W Jin W et al. Direct Desorption / Ionization of Analytes by Microwave Plasma Torch for Ambient Mass Spectrometric Analysis J. Journal of Mass Spectrometry Wan T Q Yu D D Zhang T Q et al. A Rapid Method for Detection of Gunshot Residue Using Microwave Plasma Torch-Mass Spectrometry J. Procedia Engineering Zhou W Xiong H L Yang M L et al. Microwave Plasma Torch Mass Spectrometry for Rapid Differentiation of Natural and Artificial Construction Stones J. Rock and Mineral Analysis MPT J Duan Y X Du X G Liu J et al. Determination of Zine by Microwave Plasma Torch-Atomic Fluorescence Spectrometry with Nebulization Sample Introduction System J. Chinese Journal of Analytical Chemistry

6 - 34 J Zhang H Q Liang F Zhao X J et al. An Investigation on Analytical Performance of Microwave Plasma Torch with a Pneumatic Nebulization Sample Introduction System J. Chemical Journal of Chinese Universities Li L H Zhang J S Zhang Q K et al. Determination of Calcium Magnesium and Natrium in the Mineral Water by MPT-AES J. Journal of Petrochemical Universities 24. MPT AES J Ding J H Gu H W Yang S P et al. Selective Detection of Diethylene Glycol in Toothpaste Products Using Jin Q H. A Study on Determination of Copper by Atomic Neutral Desorption Reactive Extractive Electrospray Emission Spectrometry Using Microwave Plasma Torch Ionization Tandem Mass Spectrometry J. Analytical J. Spectroscopy and Spectral Analysis MPT - AES Ca Mg Na J. Chemistry Rapid Determination of Calcium Ions in Water by Microwave Plasma Torch - Mass Spectrometry Coupled with Pneumatic Nebulization YANG Mei-ling 1 ZHONG Tao 1 2 PEI Miao-rong 1 ZHANG Xing-lei 1 LE Zhang-gao 1 WANG Guang-cai 2 CHEN Huan-wen 1* 1. Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation East China Institute of Technology Nanchang China 2. School of Water Resources and Environment China University of Geosciences Beijing Beijing China Abstract Metal element contents in water samples are commonly determined by Inductively Coupled Plasma-Mass Spectrometry ICP-MS. ICP-MS has a low detection limit and wide linear range but has a high power large gas consumption and high cost. A rapid method for the determination of calcium ions in water samples was developed by using Microwave Plasma Torch MPT -Mass Spectrometry coupled with pneumatic nebulization. The effects of carrier gas flow rate and the support gas flow rate on calcium response signal were investigated. The detection limit of this method is ng /L relative standard deviations RSDs are 1. 2% % and recoveries range from 86. 3% to %. This method avoids sample pretreatment and has a short analysis time good sensitivity and precision. This method provides a new approach for the determination of metal ions in environmental water and may be used for in situ analysis in the future. Key words water sample calcium pneumatic nebulization sampling Microwave Plasma Torch-Mass Spectrometry 591

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