间接原子吸收光谱法测定头孢克肟含量

提出了测定药物制剂中头孢克肟含量的间接原子吸收分析方法.在碱性介质中加热后,头孢克肟发生水解反应,其水解产物与酒石酸铜定量反应生成沉淀,离心分离后,利用原子吸收法通过测定沉淀中铜含量间接确定头孢克肟的含量.头孢克肟的浓度在39.7-226.7μg/mL范围内与吸光度呈良好的线性,线性相关系数r=0.9990,测定结果的...     

New Zn(Ⅱ)/M(Ⅰ)(M=Na,K and Rb) Metal-organic Frameworks Based on 5-Methylisophthalic Acid Ligand:Syntheses,Structures and Fluorescent Property

Reactions of Zn(NO3)2·6H2O and MNO3(M = Na, K and Rb) with H2mip(H2mip = 5-methylisophthalic acid) in DMF(DMF = N,N′-dimethylformamide) resulted in the formation of novel heterometallic metal-organic frameworks(Me2NH2)[ZnM(mip)2](1: M = Na; 2: M = K; 3: M = Rb, mip = 5-methylisophthalate dianion for 1~3). These complexes belong to the monoclinic system, space group P2/c and have been fully characterized by satisfactory elemental analysis, FT-IR spectra, TGA and single-crystal X-ray diffraction. Single-crystal X-ray diffraction studies reveal that 1~3 are 3D isomorphic structures based on a trinuclear unit {ZnM2(?2-COO)2(?3-COO)2} and exhibit pcu topological net and blue fluorescence.     

A New Acentric Heterometallic Inorganic-organic Hybrid Framework [ZnK_2(m-BDC)_2(H_2O)_2]n: Fluorescent,NLO and Ferroelectric Properties

Solvothermal reactions of Zn(NO3)2·6H2O with isophthalic acid in the presence of potassium nitrate lead to an acentric three-dimensional(3D) hetero-metallic inorganic-organic hybrid framework [ZnK2(m-BDC)2(H2O)2]n(1, m-H2 BDC = benzene-1,3-dicarboxylic acid). The crystal was characterized by elemental analysis, IR spectroscopy, TGA and single-crystal X-ray diffraction analysis. Complex 1 is of orthogonal crystal system, acentric space group Cmc21 with a = 19.764(6), b = 19.948(6), c = 12.039(4) , V = 4746(3) 3, Z = 4, C32H20O19K4Zn2, Mr = 995.66, Dc = 1.393 g/cm3, F(000) = 2000 and μ = 1.426 mm-1. The final R = 0.0761 and wR = 0.1841. The crystal exhibits remarkable blue luminescence emissions with high quantum yield of 56.02% and displays modest powder SHG efficiency of about 0.7 times that produced by a potassium dihydrogen phosphate(KDP) powder. In addition, it also exhibits potential ferroelectric property.     

邻羟基苯基重氮氨基偶氮苯的合成及与镉的显色反应

报道了邻羟基苯基重氮氨基偶氮苯(o-HDAA)的合成及其与镉的显色反应.在Triton X-100存在下,pH10的Na2B4O7-NaOH缓冲溶液中,该试剂与Cd(Ⅱ)形成3:1稳定的红色络合物,其最大吸收波长为516nm,表观摩尔吸光系数为1.88×105L·mol-1·cm-1,Cd(Ⅱ)浓度在0-20.0μg/25mL符合朗伯-比耳定律.用拟定方法测定废水中微量镉,结果令人满意.     

铁-抗坏血酸-3,3′,5,5′-四溴联苯-双-(重氮氨基偶氮苯)催化褪色光度法测定痕量铁

研究了在硫酸介质中 ,铁 催化抗坏血酸还原 3 ,3′,5 ,5′ 四溴联苯 双 (重氮氨基偶氮苯 )(TBDPBDAA)而褪色的反应及其动力学条件 ,测定了反应级数和表观活化能 ,建立了催化动力学光度法测定痕量铁的新方法。方法的测定范围为 0～ 0 .0 80mg L;测定下限为 4.3× 1 0 - 1 0 g mL。用于测定发样、茶叶、面粉中的痕量铁 ,与电感耦合等离子体原子发射光谱法 (ICP AES)对照 ,结果满意。     

间接原子吸收光谱法测定药物制剂中的西米替丁

本文提出了流动注射原子吸收光谱法间接测定西米替丁的新方法。基于西米替丁与Ag（I）反应可以生成白色的沉淀，经流动注射在线过滤稀释，以原子吸收光谱法测定反应剩余银离子的量来间接测定西米替丁的量。在优化条件下西米替丁浓度在2～80mg／L范围内与吸光度呈良好的线性关系，回收率为97．0％～104．3％。方法用于片剂西米替丁的测定，结果满意。     

浊点萃取-火焰原子吸收光谱法测定痕量铜

2-磺酸基-4-甲氧基苯基重氮氨基偶氮苯(MOSDAA)和Cu(II)反应生成疏水性络合物后,被萃取到Triton X-114非离子表面活性剂胶束相中,火焰原子吸收光谱法测定其中的铜,建立了浊点萃取预富集-火焰原子吸收光谱法测定铜的方法。反应体系的pH、MOSDAA和Triton X-114的浓度、平衡温度及时间等实验条件被优化。在选择的实验条件下,方法的检出限为1.1 ng/mL(3σ),对浓度为0.1μg/mL的Cu(II)溶液平行测定6次,相对标准偏差为1.9%。方法已用于小米和水样中痕量铜的测定。     

流动注射-氢化物发生-原子吸收光谱法测定海水中铅

建立了海水中铅的流动注射-氢化物发生-原子吸收光谱法。在优化的实验条件下，铅的检出限为0．1733ng／mL，线性范围为1．00-52．00ng／mL，相关系数r=0．9995。     

云冈石窟岩缝结晶物中钙离子的测定

用火焰原子吸收光谱法测定了云冈石窟岩缝结晶物中Ca的含量,为研究石窟裂缝发育病害的防治提供了一定的科学依据.样品采用5%HNO<,3>溶解,校准曲线法测定,Ca的浓度在0.004-20μg/mL范围内与吸光度有良好的线性关系,线性回归方程为A=0.0887C+0.0015,相关系数r=0.9990.相对标准偏差为1.2...