二氧化钛涂覆中空纤维膜微萃取-电热蒸发-电感耦合等离子体质谱分析环境样品中痕量重金属

采用溶胶-凝胶法制备了Ti O2涂覆中空纤维膜,并对其进行了X射线衍射和扫描电镜表征。考察了其对多种金属离子的吸附行为,最佳的萃取条件为试样的p H=8.0,在搅拌速率700 r/min下萃取30 min,使用100μL 1 mol/L HNO3进行解吸。基于此,建立了Ti O2涂覆中空纤维膜微型化固相萃取-电热蒸发（ETV）-电感耦合等离子体质谱（ICP-MS）联用测定环境水样中痕量重金属的新方法。本方法对Cr（Ⅲ）,Cu（Ⅱ）,Cd（Ⅱ）和Pb（Ⅱ）的检出限分别为0.039,0.021,0.009和0.018 ng/m L,富集倍数为10.3~18.6倍。自制Ti O2涂覆中空纤维膜的制备...

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Bibliographic Details
Published in分析化学 Vol. 43; no. 9; pp. 1313 - 1321
Main Author 王樊 何蔓 陈贝贝 向洋 胡斌
Format Journal Article
LanguageChinese
Published 武汉大学化学与分子科学学院，生物医学分析化学教育部重点实验室，武汉430072%东风商用车有限公司，东风商用车技术中心工艺研究所，十堰442001 2015
Subjects
二氧化钛涂覆中空纤维膜
固相微萃取
电感耦合等离子体质谱
电热蒸发
重金属离子
电感耦合等离子体质谱
Solid phase microextraction
Heavy metal ions
Electrothermal vaporization
重金属离子
二氧化钛涂覆中空纤维膜
固相微萃取
Inductively coupled plasma mass spectrometry
电热蒸发
Titania coated hollow fiber
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ISSN0253-3820
DOI10.11895/j.issn.0253-3820.150580

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Summary:采用溶胶-凝胶法制备了Ti O2涂覆中空纤维膜,并对其进行了X射线衍射和扫描电镜表征。考察了其对多种金属离子的吸附行为,最佳的萃取条件为试样的p H=8.0,在搅拌速率700 r/min下萃取30 min,使用100μL 1 mol/L HNO3进行解吸。基于此,建立了Ti O2涂覆中空纤维膜微型化固相萃取-电热蒸发（ETV）-电感耦合等离子体质谱（ICP-MS）联用测定环境水样中痕量重金属的新方法。本方法对Cr（Ⅲ）,Cu（Ⅱ）,Cd（Ⅱ）和Pb（Ⅱ）的检出限分别为0.039,0.021,0.009和0.018 ng/m L,富集倍数为10.3~18.6倍。自制Ti O2涂覆中空纤维膜的制备重现性（RSD）为4.5%~6.8%（批内）和7.7%~9.6%（批间）。本方法被成功应用于标准水样、东湖水和雪水中Cr（Ⅲ）,Cu（Ⅱ）,Cd（Ⅱ）和Pb（Ⅱ）的分析。另外,将Ti O2涂覆中空纤维膜与Ti O2涂覆中空纤维膜搅拌棒进行了比较,结果表明,Ti O2涂覆中空纤维膜不仅制备简单,而且对目标金属离子具有较高的萃取效率和吸附容量。
Bibliography:TiO2 coated hollow fiber （HF） was prepared by sol-gel method and characterized by X-ray powder diffraction and scanning electron microscope. The adsorption performances of the self-prepared TiO2 coated HF for interest metal ions were explored. The sample solution was extracted for 30 rain at pH 8.0 under stirring at speed of 700 r/min, then desorpted with 100 μL of 1 mol/L HNO3. On the basis of this, a method combining TiO2 coated HF micro-solid phase extraction with electrothermal vaporization-inductively coupled plasma mass spectrometry （ICP-MS） was developed for the determination of trace metal ions in environmental water samples. Under the optimized conditions, the limits of detection obtained by the proposed method were 0. 039, 0.021,0.009 and 0.018 ng/mL for Cr（Ⅲ）, Cu（Ⅱ）, Cd（Ⅱ） and Pb（Ⅱ） with enrichment factors of 12.5, 11.7, 10.3 and 18.6, respectively. The preparation reproducibility of self-prepared TiO2 coated HF ranged from 4.5% to 6.8% （n = 9） in one batch, and from 7.7% to 9.6% （n = 7 ） in batch-
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.150580