纳米TiO_2/SiO_2复合材料的制备及其对痕量镉的吸附性能研究
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摘要
以钛酸丁酯和硅酸乙酯为主要原料,制备多孔纳米TiO2/SiO2复合材料,并对其进行了电镜扫描、红外光谱、氮吸附-脱附等表征.在pH=7.5、流速为1.2mL/min的条件下,试液中的痕量镉可被纳米TiO2/SiO2复合材料定量吸附,其动态饱和吸附容量为30.0mg/g,吸附在复合材料上的镉可用1.0mol/L HCl洗脱,洗脱液中的镉用火焰原子吸收法测定.该方法的检出限为15.2μg/L,线性范围为0.05～2.5mg/L,相对标准偏差为2.6%,加标回收率在96.0%～106.5%之间.方法应用于环境水样中痕量镉的测定.
Nano TiO2/SiO2 composite as a new sorbent was synthesized with tetrabutyl titanate and ethyl silicate and characterized using scanning electron microscope(SEM),infrared spectrum(IR) and Nitrogen adsorption and desorption.At pH 7.5 and flow rate 1.2 mL/min,the cadmium in solution could be quantitatively adsorbed by nano TiO2/SiO2 composite and dynamic adsorption capacity was 30.0 mg/g.The adsorbed cadmium could be eluted with 1.0 mol/L HCl and the Cd2+ in eluant was determined by flame atomic absorption spectrometry.The detection limit was 15.2 μg/L,the relative standard deviation(RSD) was 2.6%,and the calibration curve was linear over Cd2+ concentration in the range of 0.05~2.5 mg/L.The spiked recoveries ranged from 96.0% to 106.5%.The method was applied for determination of trace cadmium in environmental water samples with satisfactory results.
Nano TiO2/SiO2 composite as a new sorbent was synthesized with tetrabutyl titanate and ethyl silicate and characterized using scanning electron microscope(SEM),infrared spectrum(IR) and Nitrogen adsorption and desorption.At pH 7.5 and flow rate 1.2 mL/min,the cadmium in solution could be quantitatively adsorbed by nano TiO2/SiO2 composite and dynamic adsorption capacity was 30.0 mg/g.The adsorbed cadmium could be eluted with 1.0 mol/L HCl and the Cd2+ in eluant was determined by flame atomic absorption spectrometry.The detection limit was 15.2 μg/L,the relative standard deviation(RSD) was 2.6%,and the calibration curve was linear over Cd2+ concentration in the range of 0.05~2.5 mg/L.The spiked recoveries ranged from 96.0% to 106.5%.The method was applied for determination of trace cadmium in environmental water samples with satisfactory results.
引文
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[2]李方,郑怀礼.卟啉配合物-巯基棉体系分光光度法测定中药中铅、镉、铜[J].光谱学与光谱分析,2004,24(2):197-199.
[3]李燕群.原子吸收光谱法在重金属铅镉分析中的应用进展[J].冶金分析,2008,28(6):33-41.
[4]杨国武,王明海,李杰,等.氢化物发生-原子荧光光谱法测定镀锌板镀层中痕量镉[J].冶金分析,2009,29(10):32-35.
[5]杨欣,徐玲玲,周秋兰,等.石墨烯基纳米复合物修饰印刷电极伏安法测定水中镉[J].分析测试学报,2011,30(11):1257-1 261.
[6]朱霞萍,汪模辉,李锡坤,等.阴离子交换树脂分离富集水中痕量镉[J].离子交换与吸附,2006,22(3):268-272.
[7]XIE F Z,LIN X C,WU X P,et a1.Solid phase extraction of lead(II),copper(II),cadmium(II)and nickel(II)using gallic acid-modified silica gel prior to determination by flame atomic absorption spectrometry[J].Talanta,2008,74(4):836-843.
[8]李云春,弓振斌,李俊,等.河口水体中痕量稀土元素的共沉淀预富集-电感耦合等离子体质谱法测定研究[J].分析测试学报,2005,24(1):12-16.
[9]干宁,王峰,巫远招.米面中痕量铍的微波消解-固相萃取/石墨炉原子吸收光谱法分析[J].分析测试学报,2009,28(8):940-943.
[10]周方钦,龙斯华,杨学群,等.硫化棉富集-火焰原子吸收光谱法测定水样中痕量的铅镉铜的研究[J].湘潭大学自然科学学报,2001,23(4):81-83.
[11]丁士文,董伟,王利勇,等.混晶纳米TiO2的制备及对含氰废水的降解研究[J].湘潭大学自然科学学报,2008,30(1):69-72.
[12]吕华,姜聚慧.纳米二氧化钛的制备及其在环保领域的应用[J].无机盐工业,2008,40(8):15-18.
[13]倪小敏,张小俊,蔡昕,等.TiO2/SiO2纳米介孔复合薄膜的制备及其光催化降解性能研究[J].安全与环境工程,2009,16(2):40-43.
[14]王先友,王雁生,汪形艳,等.高性能Li4Ti5O12的合成及其电化学性能研究[J].湘潭大学自然科学学报,2010,32(1):57-62.
[15]XING Q L,CHENG H L,CUI B,et al.Preparation and dielectric properties of Nb-doped barium titanate nano-powders and ce-ramics by sol-gel auto-combustion process[J].湘潭大学自然科学学报,2010,32(1):48-53.
[16]WANG W M,FU Z Y,WANG H,et al.Chemistry reaction processes during combustion synthesis of B2O3/TiO2-Mg system[J].Journal of Materials Processing Technology,2002,128:162-168.
[17]SAVA B A,ADROANA D,LUCICA B,et al.Raman and ESR study of sol-gel materials from ZnO-B2O3/TiO2system[J].Jour-nal of Non-Crystalline Solids,2009,355:2 020-2 022.
[18]CHENG P,ZHENG M P,JIN Y P,et al.Preparation and characterization of silica-doped titania photocatalyst through sol-gelmethod[J].Materials Letters,2003,57:2 989-2 994.
[19]杨秋文,刘素琴,黄可龙,等.Fe(Ⅲ)掺杂介孔TiO2的溶剂热法合成与表征[J].湘潭大学自然科学学报,2009,31(1):71-76.
[20]庞久寅,王春鹏,储富祥,等.水解法制备纳米二氧化硅和表征[J].胶体与聚合物,2007,25(3):12-14.
[21]宋宽秀,颜秀茹,霍明亮,等.TiO2-SiO2复合材料的制备和表征[J].硅酸盐通报,2000,5(2):36-39.
[22]宇海银,顾家山,关明云,等.纳米二氧化钛表面改性及表征[J].高分子材料科学与工程,2004,20(5):194-197.
[23]赵振国.吸附作用应用原理[M].北京:化学工业出版社,2005:72.
[24]魏芸,李忠全,汪俊琴,等.GB/T19587-2004,气体吸附BET法测定固态物质比表面积[S].北京:中国标准出版社,2004.
[25]朱庆山,黄文来,周素红,等.GB/T21650-2008,压汞法和气体吸附法测定固体材料孔径分布和孔隙度[S].北京:中国标准出版社,2008.