中红外光谱透射比标准物质研制

采用物化性质稳定的单晶硅作为基质,以直流磁控溅射方式轻蒸镀不同厚度的镍、铬混合膜层,实现了中红外波段(500~4000 cm^–1)不同透射比标准物质的研制。研制的中红外光谱透射比标准物质其透射比标称值分别为10%和50%,扩展不确定度优于0.008(k=2)。该标准物质具有量值稳定、光谱平坦等特点,可用于各类傅里叶变换红外光谱设备的透射比校准。     

火灾探测器滤光片校准方法

以紫外可见近红外分光光度计为计量标准器建立火灾探测器滤光片校准方法。火焰探测器紫外滤光片校准选择波长范围150~300 nm进行光谱扫描,测量滤光片在紫外区域的透射比;红外滤光片校准选择波长范围800~1 100 nm进行光谱扫描,测量滤光片在红外区域的透射比。线型光束感烟火灾探测器滤光片校准波长扫描范围设置为700~1 100 nm,取850~950 nm透射比平均值计算减光值。火焰探测器紫外滤光片校准结果为220,240,260,280 nm波长下的透射比,红外滤光片校准结果为850,900,950,1 000 nm波长下的透射比,不作合格性判定。线型光束感烟火灾探测器滤光片减光值标称值为0.4,0.9 d B时,误差不超过±0.1 d B;减光值标称值为10.0 d B时,误差不超过±1.0 d B。     

Ce3+掺杂对纳米TiO2/SiO2镀膜玻璃性能的影响

在TiO2/SiO2溶胶中按不同比例掺杂Ce3+得到复合溶胶,将溶胶喷涂在浮法玻璃原片上,105～300 ℃烘干得到镀有纳米TiO2膜的透明玻璃.AFM图像表明 掺杂Ce3+的TiO2/SiO2镀膜玻璃表面的颗粒小于没有掺杂Ce3+的TiO2/SiO2镀膜玻璃表面颗粒.掺杂Ce3+与TiO2 摩尔比为0.01∶1时,镀膜玻璃可见光透射比为85.3%,紫外线透射比39.7%、可见光反射比7.3%、太阳光直接透射比83.5%、太阳光直接反射比6.6%; 水接触角θ为0°; 在可见光照射下,分解甲基橙的时间为48 h; 膜表面电阻率为5.9×107 Ω·cm.在400～700 ℃对镀膜玻璃进行高温处理,其光学性能明显提高,可见光透射比为91.7%,紫外线透射比39.1%、可见光反射比6.4%、太阳光直接透射比92.0%、太阳光直接反射比5.9%; θ角为0°,亲水性明显提高; 在可见光照射下,甲基橙分解时间为28 h; 膜表面电阻率为5.5×107 Ω·cm,玻璃在可见光条件下就具有自清洁能力.     

二芳基肟苄醚类化合物的合成及杀菌活性

以吡啶芳酮为原料,合成了11个含二芳基肟醚结构单元的甲氧丙烯酸酯类化合物,通过氢核磁共振谱(~1H NMR)、碳核磁共振谱(~(13)C NMR)和高分辨质谱(HRMS)等方法对其结构进行了确证.离体杀菌活性测定结果表明,该类化合物对供试的7种植物病原菌普遍表现出较高的抑制活性,其中化合物5d和5g的活性与对照药剂嘧菌酯和肟菌酯相当.进一步活体盆栽验证实验结果表明,在400 mg/L浓度下,部分化合物表现出很好的防治效果,如化合物5h对小麦白粉病和黄瓜炭疽病的防治效果达100%.另外,该类化合物对稻梨孢的孢子萌发具有强烈的抑制作用,在25 mg/L浓度下,绝大多数化合物的抑制率达到100%,但对灰葡萄孢的孢子萌发普遍无效.研究结果显示该类化合物具有进一步开发的价值.     

红外分光光度计检定不确定度评定

以JJF 1059.1–2012为依据,对红外分光光度计计量检定的不确定度进行评定。分析了检定过程中波数示值误差及透射比示值误差不确定度的重要来源,包括测量重复性、标准物质等引入的不确定度分量。对各不确定度分量进行分析计算,波数示值误差测量结果的扩展不确定度U=1.1 cm–1,k=3。透射比示值误差测量结果的相对扩展不确定度U rel=0.2%,k=2。     

含氟吡啶羧酸酯类化合物的合成及生物活性

为了寻找具有生物活性的新化合物,以氟乙酸甲酯、氰乙酰胺和甲酸乙酯为起始原料,经环合、氯化、水解、酰氯化等反应合成了含氟吡啶酰氯中间体,再与醇类和酚类反应合成了一系列含氟吡啶羧酸酯类化合物,总收率约38%。其结构经1HNMR、13CNMR、IR、MS及元素分析测试技术确证。初步杀虫抑菌活性测试表明,部分化合物1e、1i、1j和1k在500mg/L浓度下,对淡色库蚊的杀死率在61.9%～100%之间,但对几种受试植物病菌的抑制活性很差。化合物1k活性最好,在500mg/L时对粘虫(armyworm)和淡色库蚊(culex mosquito)的杀死率均为100%。初步构效关系分析表明,芳杂环酚的该类化合物有较好的活性,而脂肪醇的该类化合物无活性。     

数显式分光光度计0%、100%失调的处理

介绍了数显式分光光度计 0 %、10 0 %失调的原因及处理方法     

光谱透射比标准物质的研究

研制了紫外、可见、近红外光谱区通用光谱透射比较标准物质。以高纯熔融石英为基片材料，镍铬合金的镀膜材料，采用双光楔对称光胶结构以消除同色杂散光的影响，对镀膜进行光胶处理以保证膜层的强度、稳定性及光学中性，采用高精度分光光度测量装置作为定值手段的以保证准确的定值，设计定位保护架以消除多次反射误差。该光度标准适用的光谱范围的200-2600nm，光谱透射比定值不确定度为0.5%。     

1,3,4-噻二唑基1,2,4-三唑啉酮类化合物的合成及除草活性

以2-甲基-5-氨基-1,3,4-噻二唑和芳香醛为原料,设计合成了一系列新型1,2,4-三唑啉酮类化合物。通过1H MR、MS和元素分析确证了其结构。生物活性测试结果表明,在100μg·m L-1浓度下,该类化合物具有较好的除草活性,其中化合物4c和4d对油菜和稗草的抑制率达到了80%。     

手性螺环双膦氧化物催化的不对称还原-Aldol反应(英文)

以螺环膦氧化合物为催化剂及三氯硅氢为还原剂,发展了手性Lewis碱催化的烯酮与醛的不对称还原-Aldol反应.该类催化剂在查耳酮以及类似物与各种醛的不对称还原-Aldol反应中表现出较高的反应活性和良好的立体选择性,以较好的产率(45%-88%)、中等到优秀的非对映选择性(8:92-100:0)以及最高达95%的ee值得到相应的还原Aldol产物.     

ON THE INTERPRETATION OF ABSORPTION SPECTRA OF LEAVES–I. INTRODUCTION and THE CORRECTION OF LEAF SPECTRA FOR SURFACE REFLECTION

Abstract— Reflectance and transmittance spectra of leaves and their sum can be corrected to relate only to the light actually entering the leaf, if the reflectance of the epidermal surface is known. The latter is found if the leaf reflectances at several wavelengths near the transmittance minimum in the red are plotted vs the transmittances of a homogeneous suspension of the native pigment-proteins at the same chlorophyll content per unit area and at the same wavelengths. With non-senescent leaves, the relation is linear and the extrapolation of the pigment transmittance to zero gives the value for the surface reflection. Surface reflectance data (both adaxial and abaxial) are given for the leaves of a number of trees and a few herbs, plus examples of the raw and corrected spectra. With normal, glaucous leaves, the adaxial reflectance averaged 4.5% of the incident light ( n = 23, range = 3.7 −5.9, standard deviation = 0.4). The reflectances of the abaxial surfaces ranged between 7 and 13% since additional near-surface reflection occurred at the inside of the epidermis and in the spongy mesophyll. Reflectance and transmittance data demonstrated strong absorption in the epidermis below 480 nm.     

表面活性剂辅助酸催化溶胶-凝胶法制备高强度超亲水二氧化硅减反增透纳米粒子涂层

以正硅酸乙酯(TEOS)、十六烷基三甲基溴化氨(CTAB)、盐酸(HCl)、乙醇和水为原料,通过溶胶-凝胶法提拉涂膜,再经700 ℃快速淬火200 s,制备了二氧化硅（SiO2）纳米粒子涂层。 研究了CTAB浓度、提拉速度、停留时间和提拉涂膜次数对透射率的影响,结果表明,当CTAB质量分数为2.5%,提拉速度为100 mm/min,停留时间为60 s,提拉涂膜1次得到的SiO2纳米粒子涂层透射率最高,可达95.9%。 该涂层具备超亲水性并能耐受6H铅笔刮痕测试。 实验还表明,在SiO2溶胶液中加入CTAB,通过其与TEOS部分水解生成的物种的相互作用,可以改善酸性催化条件下形成的SiO2溶胶的微观结构,从而提高了涂层的透射率和亲水性。     

Anti-scratch and transparency properties of transparent conductive carbon nanotube films improved by incorporating polyethoxysiloxane

Transparent conductive films of single-walled carbon nanotubes (SWCNTs) were fabricated by a simple method to significantly enhance anti-scratch and transparency properties by the incorporation of polyethoxysiloxane (PES). The reasons for changes in the mechanical properties and transmittance were investigated through the reflection property and morphology of thin films. With the incorporation of PES, the sheet resistance of the SWCNT thin film remained unchanged after the anti-scratch test. It was found that the transmittance of the thin films suddenly increased when the thickness of the PES layer was ca 100 nm. Although the PES incorporation resulted in a slight increase in the sheet resistance, the experimental results revealed that the sheet resistance of the SWCNT thin films with PES was lower than that of films without PES for the same transmittance due to the increase of the transmittance caused by the PES incorporation. We have demonstrated that the sheet resistance was halved at a transmittance of ～86% due to PES incorporation. SWCNT thin films with PES showed better electrical properties than those without PES after a bend test.     

ON THE INTERPRETATION OF ABSORPTION SPECTRA OF LEAVES–II. THE NON-ABSORBED RAY OF THE SIEVE EFFECT and THE MEAN OPTICAL PATHLENGTH IN THE REMAINDER OF THE LEAF

Abstract— The sieve effect and scattering within leaves are analysed by the use of a simple model. By plotting the leaf transmittance (corrected for light not entering the leaf) vs the transmittance of an equivalent amount of homogeneous plastid pigments, an intercept is found where the latter is zero. This minimum transmittance represents the fraction of the leaf area devoted to the ray of the sieve effect which strikes no chloroplasts. It varied between 7% and 0.2% in non-senescent leaves. When this was subtracted from the leaf spectrum, the peak absorbance was greater than that of the homogeneous leaf pigments in all cases. The ratio of the leaf absorbance to that of the homogeneous pigments, at the same wavelength, is the apparent optical pathlength, which increases with decreasing absorbance. By plotting this ratio vs the absorbance of the equivalent homogeneous pigment, an intercept is found where the latter is zero. This intercept is interpreted as an estimate of the true mean scattering pathlength. Leaves with high chlorophyll contents had low pathlengths (mean and SD = 2.30 ± 0.25); with moderate and low contents, the values were higher (2.75 ± 0.28, 3.95 ± 0.77). Another application of the model gave values between 3 and 4 for the true scattering pathlength.     

具有高散射能力的聚碳酸酯复合材料的制备与性能研究

以双酚A型聚碳酸酯(PC)为基体、苯乙烯-丙烯腈共聚物(SAN)为散射体,通过熔融共混方法制备了同时具备高透光率和高雾度的高散射聚碳酸酯光散射片,研究了SAN含量对光散射片微观结构和光散射性能的影响,发现透光率和雾度同时随着散射体含量增加而提高的现象.研究结果表明,当SAN含量低于30%时,分散相为球形颗粒,颗粒的平均粒径随着SAN含量的增加而增加,而颗粒的数量浓度则随之减小,这使得其透光率和雾度均随着SAN含量的增加而增加,当SAN含量为30%时,透光率和雾度达到最大值,分别为89.1%和91.7%.并结合Mie散射理论解释说明了透光率和雾度同时随着散射体含量的增加而提高的现象.但当SAN含量的进一步增加,分散相颗粒尺寸已远大于光波的波长,不再适用于Mie散射理论,且部分不再呈球形颗粒,使得PC片的透光率和雾度略有降低.     

具有光导性的磁性高分子粒子的合成与表征

采用分散聚合法合成了表面带羟基、内核为四氧化三铁的磁性高分子粒子 ,再用酯化法在粒子表面共价结合有机光导分子酞菁 ,得到了同时具有光导性和磁响应性的磁性高分子粒子     

全差示光度法三大参数的相互关系及其应用

本文介绍全差示法调百参比T_r、反向微电流i、标尺放大倍数x的定义和性质,导出调零参比T_R,论述了参数间相互关系。用计算机绘制不同x的相对误差函数图。用全差示法测定磷矿样品的P_2O_5含量,结果良好。     

Spectroscopic Investigations of Phase-Separated Thermotropic Layers Based on UV Cured Acrylate Resins

Summary: In this paper spectroscopic techniques were adapted and applied to characterize the optical and morphological properties of thermotropic resins. Thermotropic films were prepared by variation of resin base and thermotropic additives. By UV/Vis/NIR spectroscopy the solar optical properties, the switching temperature, the switching process and the residual transmittance in the opaque state were determined. To control the sample temperature from ambient to 100 °C a conventional UV/Vis/NIR spectrophotometer equipped with an Ulbricht-sphere was adapted by a heating stage. Additive content, distribution and scattering domain size were characterized by Differential Scanning Calorimetry, Attenuated Total Reflectance spectroscopy and microscopic techniques. For the investigated film types hemispheric solar transmittance values ranging from 80 to 87% and 75 to 85% were obtained in the clear and the scattering state, respectively. The diffuse solar transmittance values increased significantly from 14 to 40% below the switching temperature to 36 to 70% at elevated temperatures. The thermotropic resins exhibit a steep and rapid switching process with switching temperatures between 45 and 70 °C. The materials with the best switching properties are characterized by distinct differences in refractive index between the components, a uniform additive distribution and scattering domains with diameters below 1000 nm.     

聚醚砜单烯大分子单体的合成与表征及其共聚物的光学特性

本文采用溶液法以单酚（４－氯－４’－羟基二苯砜）为原料合成了不同聚合度的单酚低聚体，得到了控制聚合度的最佳聚合条件；用相转移催化剂法成功地将单酚转化为单烯大分子单体，并用ＩＲ、１Ｈ—ＮＭＲ对其结构进行了表征；测定了双键官能度均在１．９０以上．单烯大分子单体与苯乙烯的共聚研究表明，聚合度为２左右的单烯大单体在苯乙烯中溶解度最大，可达８０％以上；共聚物有优异的光学特性，对折射率的提高比相应的双烯大分子单体有利；在可见及近红外区透光率达８９％以上．