红外镜反射光谱的测试与解析

红外镜反射（infrared specular reflection，简称SR）光谱与被测样品和衬底的折射指数、吸收指数以及入射角有密切关系，往往由之产生畸变。要从红外镜反射技术测得的光谱处理得到人们熟悉的吸收光谱，需要经过较复杂的计算机数学处理。本文通过几个比较特殊的镜反射例子，以说明镜反射光谱的测试和解析必须注意多种影响因素。     

流动注射-氢化物发生-原子吸收光谱法测定雪中的微量铅

建立了测定雪中微量铅的流动注射-氢化物发生-原子吸收光谱法。在优化条件下。测定铅的线性范围为0～52．0ng／mL，线性回归方程为A=0．018c 0．016，相关系数r=0．9995，检出限为0．2ng／mL。用于雪中微量铅的测定，加标回收率为94．2％～107．3％，相对标准偏差为1．47％～3．22％。该方法的测定结果与标准加入法基本一致。     

Human insulin and desamido human insulin isotherms in ethanol-water reversed phase systems

The multi-component isotherms for human insulin (HI) and desamido human insulin (dHI) over reversed phase packing (C18) and with 29.8% (w/w) ethanol-water as mobile phase have been determined experimentally. The isotherms of HI in ethanol-water differ from those obtained with the more commonly applied methanol-water and acetonitrile-water mobile phase, as described in this paper. The isotherm exhibits anti Langmuirian behavior and can be very well modeled by an anti Langmuir isotherm presented in this paper. The HI and dHI anti Langmuir isotherm are determined as: qHI = (8.4C(HI) + 3C(HI)CdHI)/(1 - 0.05C(HI) - 0.14CdHI + 0.04C(HI)CdHI) and qdHI = (11.4CdHI + 2C(HI)CdHI)/ (1 - 0.05C(HI) - 0.14CdHI + 0.04C(HI)CdHI)     

Thermal decomposition of the composite hydrotalcites of iowaite and woodallite

The thermal stability and thermal decomposition pathways for synthesized composite iowaite/woodallite have been determined using thermogravimetry analysis in conjunction with evolved gas mass spectrometry. Dehydration of the hydrotalcites occurred over a range of 56–70°C. The first dehydroxylation step occurred at around 255°C and, with the substitution of more iron(III) for chromium(III) this temperature increased to an upper limit of 312°C. This trend was observed throughout all decomposition steps. The release of carbonate ions as carbon dioxide gas initialised at just above 300°C and was always accompanied by loss of hydroxyl units as water molecules. The initial loss of the anion in this case the chloride ion was consistently observed to occur at about 450°C with final traces evolved at 535 to 780°C depending of the Fe:Cr ratio and was detected as HCl (m/z=36). Thus for this to occur, hydroxyl units must have been retained in the structure at temperatures upwards of 750°C. Experimentally it was found difficult to keep CO₂ from reacting with the compounds and in this way the synthesized iowaite-woodallite series somewhat resembled the natural minerals.     

毛细管电泳安培检测扑热息痛及其水解物

研究了各种电化学预处理条件下碳纤维电极对扑热息痛及水解物的电化学行为。确定该体系最佳预处理条件为０．２Ｖ电位下阳极化１ｍｉｎ，再于－２．０Ｖ下阴极化１０ｓ。预处理后的碳纤维伏安响应得到明显提高。运用最佳条件并在支持电解中加入添加剂后，扑热息痛及其水解物在毛细管电泳上获得很好的分离和检测。其中扑热息痛的检测下限为２．７８ｐｇ；对氨基酚为１．８４ｐｇ。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

VA族元素对阳极铅(Ⅱ)氧化物膜半导体性质的影响(Ⅱ)

用光电化学电流法研究了铅、铅砷、铅锑和铅铋合金在4．5mol·L－1H2SO4溶液（22℃）中，以0．9V（vs．Hg／Hg2SO4）极化7h而形成的阳极膜中的氧化铅的半导体性质，合金添加剂砷、锑和铋对t－PbO（四方氧化铝）和o-PbO（斜方氧化铝）的禁带宽度没有影响，从量子效率和电位的关系可求Pb，Pb－lat％As（at％表示原子百分比，全文同），Pb-lat％Sb和Sb－lat％Bi上膜中t－Pbo的施主密度（ND）分别为9．3×1015，1．0×1016，3．1×1016和1．3×1017cm-3，平带位分别为-0．20，－0．22，－0．28和-0．08V（vs．Hg／Hg2SO4）．比较VA元素砷、锑和铋对上述膜中t－Pbo的ND（从而自由电子密度）和膜中t－Pbo的生长速率的影响，可认为法添加剂砷、锑和铋对阳极膜中t-Pbo的作用符合Hauffe规则．     

无相移滤波技术用于分析化学信号处理

把无相移滤波技术引入了分析化学信号处理领域。其方法为：先将输入序列按顺序滤波，然后将所得结果逆转后反向通过滤波器，再将所得结果逆转后输出。通过对色谱信号的实验研究表明，与普通的数字滤波方法相比较，无相移滤波不但具有普通数字滤波的优点，而且不会产生滤波前后的相位偏移，具有良好的应用前景，尤其对于需要准确计算保留时间的场合，用此预处理方法非常适合。     

Mesoporous micelle templated silica with incorporated C<Subscript>8</Subscript> and C<Subscript>18</Subscript> phase

Mesoporous silica material of MCM-41 type was synthesized by co-condensation of highly concentrated octyltriethoxysilane (OTEOS), octadecyltriethoxysilane (ODTEOS) and tetraethoxysilane (TEOS). The obtained hybrid materials were characterized using XRD, TG-DSC and low temperature adsorption/desorption of nitrogen. It was shown that the applied method of synthesis allows to obtain silica of MCM-41 type with a high degree of hydrocarbon saturation.