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1,8-二羟基蒽醌键合硅胶:作为固相萃取剂用于火焰原子吸收光谱法测定铅(II)、锌(II)和镉(II)之前的合成与应用。

1,8-Dihydroxyanthraquinone anchored on silica gel: synthesis and application as solid phase extractant for lead(II), zinc(II) and cadmium(II) prior to their determination by flame atomic absorption spectrometry.

机构信息

Department of Chemistry, Indian Institute of Technology, New Delhi 110016, India.

出版信息

Talanta. 2002 Oct 16;58(4):669-78. doi: 10.1016/s0039-9140(02)00374-0.

Abstract

A new chelating matrix has been prepared by immobilizing 1,8-dihydroxyanthraquinone (DHAQ) on silica gel modified with (3-aminopropyl)triethoxysilane. After characterizing the matrix with thermogravimetric analysis (TGA), cross polarization magic angle spinning (CPMAS) NMR and diffuse reflectance infrared fourier transformation (DRIFT) spectroscopy, it has been used to preconcentrate Pb(II), Cd(II) and Zn(II) prior to their determination by flame atomic absorption spectrometry. The optimum pH ranges for quantitative sorption are 6.0-7.5, 7.0-8.0 and 6.0-8.0 for Pb, Zn, and Cd, respectively. All the metal ions can be desorbed with 2 mol l(-1) HCl/HNO(3). The sorption capacity of the matrix has been found to be 76.0, 180.0 and 70.2 mumol g(-1) for Pb, Zn and Cd, respectively, with the preconcentration factor of approximately 200. The limits upto which electrolytes NaNO(3), NaCl, NaBr, Na(2)SO(4), Na(3)PO(4) sodium citrate, EDTA, glycine and humic acid and cations Ca(II), Mg(II), Cu(II), Co(II), Ni(II), Mn(II) Al(III), Cr(III) and Fe(III) can co-exist with the metal ions during their sorption without any adverse effect are reported. The lowest concentration of metal ions for quantitative recovery is 5.0 ng ml(-1) The simultaneous enrichment and determination of all the metals is possible if total load of metal ions is less than sorption capacity. The flame AAS was used to determine these metal ions in underground, tap and river water samples (relative standard deviation (R.S.D.)</=6.3%) after their enrichment with the present matrix.

摘要

一种新的螯合基质已经通过将 1,8-二羟基蒽醌(DHAQ)固定在经过(3-氨丙基)三乙氧基硅烷改性的硅胶上来制备。在用热重分析(TGA)、交叉极化魔角旋转(CPMAS)NMR 和漫反射红外傅里叶变换(DRIFT)光谱对基质进行表征后,它已被用于在火焰原子吸收光谱法测定之前预浓缩 Pb(II)、Cd(II) 和 Zn(II)。定量吸附的最佳 pH 范围分别为 6.0-7.5、7.0-8.0 和 6.0-8.0,用于 Pb、Zn 和 Cd。所有金属离子都可以用 2 mol l(-1) HCl/HNO(3) 洗脱。该基质的吸附容量分别为 76.0、180.0 和 70.2 umol g(-1),对于 Pb、Zn 和 Cd,预浓缩因子约为 200。电解质 NaNO(3)、NaCl、NaBr、Na(2)SO(4)、Na(3)PO(4) 、柠檬酸钠、EDTA、甘氨酸和腐殖酸以及阳离子 Ca(II)、Mg(II)、Cu(II)、Co(II)、Ni(II)、Mn(II)、Al(III)、Cr(III) 和 Fe(III)在不产生任何不利影响的情况下与金属离子共存的电解质的最大浓度报告为 5.0 ng ml(-1)。如果金属离子的总负载小于吸附容量,则可以实现所有金属的同时富集和测定。用本基质富集后,火焰 AAS 可用于测定地下水、自来水和河水样品中的这些金属离子(相对标准偏差(R.S.D.)</=6.3%)。

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