基于荧光光谱技术对常用洗衣粉中表面活性剂含量的测定

十二烷基苯磺酸钠(Sodium Dodecyl Benzene Sulfonate,SDBS)是一种通用的阴离子表面活性剂,其洗涤性能优良,配伍性能好,可与其他无助剂以不同比例配比,且价格便宜,被广泛应用于洗衣粉中。应用FS920荧光光谱仪分析了不同浓度的十二烷基苯磺酸钠水溶液和不同品牌洗衣粉水溶液的荧光光谱特性,发现十二烷基苯磺酸钠溶液的荧光特征峰位于λ_(ex)/λ_(em)=315/350nm,洗衣粉水溶液的荧光特征峰位于λ_(ex)/λ_(em)=356/430nm,经分析是由于洗衣粉中添加了其他非离子表面活性剂、沸石等物质使特征峰发生红移。根据荧光强度与浓度的关系,采用径向基神经网络完成了水溶液中十二烷基苯磺酸钠含量的定量测试,同时通过采用荧光光谱技术和径向基神经网络相结合的检测方法分析了生活中常见的7个常用品牌洗衣粉中表面活性剂的含量。     

FTIR光谱方法对比分析少年和老年软骨成分含量

利用傅里叶变换红外(FTIR)光谱方法测量了少年和老年人软骨的红外光谱。由OMNIC 5.2软件计算了软骨中主要有机成分(胶原)和无机成分相关光谱带的积分面积。对代表有机物和无机物的某些谱带面积大小进行了比较。结果表明：软骨中有机成分(酰氨Ⅰ)含量与无机成分(PO3-₄)含量之比少年是老年人的5～7倍;然而脂类含量却有很大的不同, 对脂类(1 747 cm-1)与无机物(PO3-₄)的谱带积分面积进行比较,老年人软骨中脂类含量明显高于少年。作者认为人体随着年龄的增加,全身性的退化在软骨中的总体表现为有机成分(胶原)的减少(而脂类含量却增加)和无机成分(磷酸盐、碳酸盐等)相对的增加,使得软骨骨质变脆,失去过多弹性,耐磨性减低,是进一步容易导致骨病和骨伤的原因。     

草酸反萃取法直接沉淀负载铈有机相的表征分析

研究了氢氧化钠介质皂化条件下,用草酸溶液从负载铈的P507有机相中直接反萃取沉淀铈的试验结果。利用红外光谱(IR)、X射线衍射(XRD)、扫描电子显微镜(SEM)及热重-差热分析仪(TG-DSC)等手段,对反萃所得铈沉淀物及最终焙烧产物的物相、形貌和热失重等进行了分析、测试与表征。实验结果表明:沉淀有机相为球形有机铈的配合物,焙烧产物为球形的立方晶系的CeO2晶体,说明前驱物与产物形貌有遗传继承性。IR证实了萃合物的结构与最终CeO2晶体结构完全不同,热重表明吸附水失重为3.5%,所得最终产物的化学组成为CeO2.1/3H2O。     

无机纳米氧化铝/聚酰亚胺复合膜的表征

研究无机纳米掺杂有机复合薄膜力学性能、热学性能、电学性能变化规律的关键在于快速、准确地掌握复合膜中纳米无机物的掺入量及其颗粒大小和分布状态。文章通过X射线荧光光谱、红外光谱、扫描电子显微镜、原子力显微镜等测试方法对无机纳米氧化铝/聚酰亚胺复合薄膜的三氧化二铝掺入量、化学结构及表面形貌进行了表征分析(该材料为本研究室制备的)。结果表明:聚酰亚胺有机相与三氧化二铝无机相之间形成了键联型复合杂化体系;三氧化二铝粒子呈纳米级均匀地分散在聚酰亚胺基体中,颗粒直径均在50nm以下;利用X射线荧光光谱法测定出三氧化二铝的质量含量为7·9%,利用该方法定性、定量分析无机纳米掺杂有机复合薄膜材料中的无机组分具有样品不需要预处理、不需要加载电荷(可用于分析绝缘材料)、非接触性、非破坏性、速度快、准确度高等优点。     

膨润土的短碳链季铵盐改性研究

以自制的钠基膨润土为原料、用四甲基氯化铵和四丁基氯化铵作为有机插层剂与膨润土层间的Na+交换, 制备出有机膨润土, 并经红外光谱分析(IR)、差热分析(DTA)和X-ray衍射分析(XRD)等测试手段对其结构进行表征。讨论了不同的季铵盐对有机膨润土性能的影响。实验表明,表面活性剂离子进入膨润土晶片层间,使其晶片层间的亲水环境改变为疏水环境以及增大晶片层间距离,增加膨润土与有机相的相容性, 为制备高聚物/膨润土纳米复合材料奠定基础。     

不同比例有机无机肥配施条件下黑土富里酸荧光光谱特征

富里酸(FA)是土壤腐殖质的重要组成成分,是土壤腐殖化过程中的中间物质,其结构特性对提高土壤有机质具有重要的指示作用。有机无机肥配施是实现土壤培肥、秸秆资源利用、减少无机肥施用的有效措施。为探讨黑龙江省黑土区秸秆有机肥替代无机肥对土壤FA的影响,设置不施肥(CK)、单施无机肥(NPK)、有机肥替代无机氮肥25% (NPKM1)、有机肥替代无机氮肥50% (NPKM2)、有机肥替代无机氮肥75% (NPKM3)及有机肥替代无机氮肥100% (NPKM4)6个处理,测定土壤有机碳(SOC)和FA含量。利用荧光指数(FI)、自生源指数(BIX)表征土壤FA的来源,腐殖化指数(HIX)指示土壤的腐殖化程度。采用三维荧光光谱-平行因子分析法,分析土壤FA的荧光组分及最大荧光强度(F_max),并利用冗余分析(RDA)探讨荧光强度、土壤有机碳和试验处理间的响应关系。结果表明：与NPK处理相比,有机无机肥配施处理均显著提高了SOC和土壤FA含量,其中对NPKM2处理影响最大,SOC含量提高8.06%,土壤FA含量提高13.84%。土壤FA受自生源和外生源共同作用的影响(FI>1.4,0.8F_max值先升高后降低,类蛋白质F_max值逐渐降低。NPKM2处理类富里酸和类胡敏酸的F_max值最高,类富里酸的相对百分比最高。RDA结果表明NPKM2处理对SOC、土壤FA含量和F_max值的影响最大。因此,基于土壤FA荧光光谱特性分析可知,为提高土壤有机质含量、增加秸秆利用率、减施无机肥,秸秆有机肥替代无机氮肥50%处理为最佳有机无机肥配比。     

砂姜黑土有机无机复合体结构特征及其对土壤颜色的影响机制

土壤颜色是反映土壤发生、形成环境及肥力特征的一项重要物理性状。通常高有机质含量土壤的颜色比较黑,但我国典型低有机质含量的砂姜黑土土壤颜色也很黑。基于传统化学方法的研究认为高度芳构化的腐殖质成分与土粒结合使砂姜黑土呈现黑色。然而采用化学方法只能提取部分腐殖质成分,且破坏了有机质及有机无机复合体的化学结构,其结果不具有代表性。通过不破坏土壤有机无机复合体结构的物理方法从砂姜黑土中提取黑色物质的研究发现蒙皂石吸附有机质形成的黑色有机无机复合体是砂姜黑土呈现黑色的决定性成分。但是,这些黑色有机无机复合体的有机质结构及复合体呈现黑色的机制还不清楚。本研究旨在通过物理方法从砂姜黑土中提取黑色组分,从有机质结构及其与蒙皂石矿物作用方面研究这些黑色有机无机复合体的特征,探讨其呈现黑色的机理。首先采用物理方法从黄淮海平原三个地点的典型砂姜黑土表土层(0～40 cm)土壤中提取浅色组分[53μm颗粒、白(W)和浅白(LW)]和黑色组分[浅黑(LB)、黑(B)和纳米黑(NB)]。然后采用分光测色仪、固态~(13)C核磁共振谱仪和X射线衍射仪分别测定不同提取组分的黑度、有机质结构和蒙皂石含量。相关分析和通径分析结果表明,提取组分有机质的羧基碳、氨基碳、烷基碳和烷氧碳对砂姜黑土黑度的直接影响效应和间接效应都较大,芳香碳含量和芳香度对土壤黑度的影响则较小,蒙皂石对土壤黑度的直接影响效应及其通过羧基碳、氨基碳和烷基碳对土壤黑度的间接效应都较大。因此,砂姜黑土中大量存在的蒙皂石通过吸附有机质中含有生/助色团的羧基碳、氨基碳、烷氧碳及烷基碳形成有机-无机复合体是其呈现黑色的主要机制,并不是传统观点认为的芳香碳及高芳香度。     

O2/CO2燃烧方式下煤中有机/无机硫的释放特性

首先用重液浮选将一种烟煤分为高(＞2.0 g/cm3)、中(1.4～2.0 g/cm3)和低(＜1.4 g/cm3)三个密度段,并采用三态硫化学分析,发现无机硫(外在黄铁矿为主)主要赋存于高密度煤中,有机硫主要赋存于低密度煤中,几乎全部硫酸盐硫、部分有机硫和少量无机硫(内在黄铁矿)赋存于中密度煤中.其次在程序升温条件下研究了分密度煤中硫的释放特性以及含硫物相的浓度变化规律,探讨了有机/无机硫析出特性的影响机理.结果显示:在O2/CO2气氛下,高、中密度煤SO2析出曲线都有尖峰并呈双峰分布,在较短时间及较窄温度范围反应完全;与之相反,低密度煤释放曲线平坦且无明显峰,在较长时间和较宽温度范围均有析出;相对于O2/N2气氛,O2/CO2燃烧方式促进了硫以COS/SO3等物相生成,同时提高了煤灰中矿物质自固硫能力,从而降低了SO2的排放.     

有机-无机杂化铜（Ⅰ）基卤化物闪烁体研究进展

近年来,有机-无机杂化金属卤化物材料由于其优异的光电性质引起了研究人员的广泛关注。其中低维铜(Ⅰ)基卤化物作为高效发光材料的代表,在照明与显示、辐射探测等领域表现出良好的应用前景。有机无机杂化铜(Ⅰ)基卤化物的组成和结构丰富多变,给研究人员提供了巨大的研究空间。本文综述了有机-无机杂化铜(Ⅰ)基卤化物作为发光材料的研究进展,并以[CuX_n](X=Cl,Br,I)结构单元及其连接方式为依据,对离子型有机-无机杂化铜(Ⅰ)基卤化物进行了系统的分类,总结了其组成-结构-性质之间的构效关系。讨论了有机-无机杂化铜(Ⅰ)基卤化物的发光机制和光物理过程,并重点归纳了用于X射线探测的有机-无机杂化铜(Ⅰ)基卤化物闪烁体的最新进展。最后,对这一新兴的研究领域做出了展望。     

电解有机溶液法在Si表面制备类金刚石薄膜及退火对其结构的影响

在对不同有机溶剂分子结构分析的基础上,选取甲醇、DMF(N,N-二甲基甲酰胺)和乙腈溶液为碳源,以脉冲直流电源电解有机溶液的方法在Si片上制得了含氢类金刚石薄膜(DLC薄膜),并研究了退火对薄膜结构的影响.通过X射线光电子能谱(XPS),喇曼(Raman)和红外(IR)光谱对薄膜的结构进行了分析表征.XPS表明薄膜的主要成分为C,喇曼光谱显示所得薄膜为典型DLC薄膜.喇曼和红外光谱还表明,膜中含有大量H并且主要键合于sp³碳处.随着退火的进行薄膜中的H被去除.随温度升高薄膜电阻率的下 关键词： 类金刚石薄膜 退火     

表面活性剂存在时氯化钠对甲苯胺蓝聚合状态的影响

本文应用紫外-可见吸收光谱研究了甲苯胺蓝在十二烷基苯磺酸钠中的聚合状态，分析了有表面活性剂存在下氯化钠对甲苯胺蓝解聚作用的影响。结果表明，无机盐促使十二烷基苯磺酸钠提前形成胶束(预胶束)，造成甲苯胺蓝二聚体的解聚。     

MPT-AES测定奶粉中的微量金属元素

用微波等离子体(MPT)为激发光源,氩气为等离子体工作气体,用气动雾化进样,以校准曲线法研究了微波等离子体炬原子发射光谱法(MPT-AES)测定奶粉中的镁、钠。详细考察了溶液中盐酸浓度、硝酸浓度、共存离子浓度、微波前向功率、载气流量、工作气流量等实验参数对测定的影响。测定结果表明,镁和钠质量浓度的检出限分别为0.36、0.75μg/L,RSD(n=6)≤0.41%,线性范围分别为0.02—9mg/L、0.02—4mg/L,MPT-AES提高了测定奶粉中微量金属元素含量的速度和准确度。     

Characterization of compositional particles in eye shadow powder by scanning electron microscope and X-ray mapping

We developed an analysis method to evaluate the size and shape of particles of eye shadow cosmetics by applying the scanning electron microscopy (SEM) combined with the energy-dispersive spectroscopy (EDS). Backscattered electron (BE) and X-ray mapping images from the SEM-EDS measurements were interpreted to identify the size and shape of powder particles according to different factors such as 9 size and 5 shape indices established in this work. By using the developed method, we could classify the inorganic and organic particles of the eye shadow powder by composition, which can contribute to improving the product quality.     

Solvent-controlled syntheses of Ni12P5 and Ni2P nanocrystals and photocatalytic property comparison

Nickel phosphide nanocrystals with various phases have been successfully synthesized via a simple solvothermal route at 180 °C for 16 h, employing nickel chloride and white phosphorus (WP) as starting reactants in the presence of sodium dodecylbenzene sulfonate (SDBS). X-ray powder diffraction (XRD) research showed that the pure Ni₁₂P₅ phase with a high yield could be obtained in an ethanol solution, and the pure Ni₂P form was prepared in a mixed system with the volume ratio of water/ethanol of 10:10. Namely, the presence of water molecules induced the phase conversion of nickel phosphides. Furthermore, in order to investigate the correlation between properties and phases, as a case, the photocatalytic degradation abilities of two nickel phosphide phases for organic dyes were compared.     

原子吸收光谱法测定婴幼儿奶粉中铁含量不确定度的评定

建立了原子吸收光谱法测定婴幼儿奶粉中铁含量不确定度评定的数学模型,分析了检测过程中不确定度来源并计算了各不确定度分量,得出合成标准不确定度和扩展不确定度。在婴幼儿奶粉中铁含量的测定中,测量值为8.156mg/100g,其扩展不确定度为0.11mg/100g,k=2。影响铁含量测量结果不确定度的最大因素是校准曲线拟合引入的不确定度。     

Syntheses and characterization of Sr(OH)2 and SrCO3 nanostructures by ultrasonic method

The Sr(OH)₂ and SrCO₃ nanostructures were synthesized by reaction of strontium(II) acetate and sodium hydroxide or tetramethylammonium hydroxide (TMAH) via ultrasonic method. Reaction conditions, such as the concentration of the Sr²⁺ ion, aging time, power of the ultrasonic device and alkali salts show important roles in the size, morphology and growth process of the final products. The pure crystalline SrCO₃ were obtained by heating of product at 400 °C. The Sr(OH)₂ and SrCO₃ nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), thermal gravimetric (TG), differential thermal analyses (DTA) and the infrared spectroscopy (IR).     

Primary release and transformation of inorganic and organic sodium during fast pyrolysis of sodium-loaded lignin

This study employs a wire-mesh reactor (WMR) to understand the primary release and transformation of inorganic and organic sodium during fast pyrolysis of various sodium-loaded lignin samples at 300–800 °C. Due to the minimization of volatile-char interactions in WMR, the overall sodium release during lignin pyrolysis is relatively low, i.e., ∼9–11% and ∼7–14% for the inorganic and inorganic sodium loaded lignin, respectively. The presence of the inorganic sodium in the condensed volatiles (so-called oil) clearly indicates the important role of thermal ejection in the release of the inorganic sodium, since sodium salts are unlikely to evaporate under current conditions. While the release of the organic sodium into oil can be due to both thermal ejection of aerosols and evaporation of low carboxylates. Despite the low sodium release, significant transformation of the inorganic and organic sodium can take place during lignin pyrolysis. For the inorganic sodium loaded lignin, the inorganic sodium decreases continuously from ∼67% at 300 °C to ∼42% at 800 °C, accompanied by a steady increase in the organic sodium (i.e., the ion-exchangeable sodium) from ∼17% at 300 °C to ∼37% at 800 °C. While for the organic sodium loaded lignin, its transformation into the inorganic sodium is faster at higher temperatures, leading to a large increase in the inorganic sodium (i.e., carbonates) from ∼9% at 300 °C to ∼48% at 800 °C, as well as a reduction in the organic sodium from ∼79% at 300 °C to ∼28% at 800 °C. The data generated in this study will be important to understand the catalytic mechanism of sodium during thermochemical processing of alkali lignin for the production of bioenergy and biofuels.     

Surface chemical modification of fullerene by mechanochemical treatment

In this study different encapsulating agents have been used for chemical modification of fullerenes. Fullerenes have reacted with tetrahydrofuran, sodium dodecyl sulfate, sodium dodecylbenzene sulfonate and ethylene vinyl acetate-ethylene vinyl versatate at room temperature under mechanical milling. The obtained powder has been dispersed in water by ultrasonication. The fullerene based colloids have been characterized by UV-vis, FTIR, Raman spectroscopy and atomic force microscopy. FTIR and Raman analysis have shown the presence of C₆₀ after surface functionalization.     

基于红外指纹图谱的螺旋藻品质分析和蛋白含量测定

采用傅里叶变换红外光谱(FTIR)分析技术,对螺旋藻标准品、螺旋藻粉样品和糊精标准品的红外光谱进行分析。螺旋藻中的蛋白质(1 657,1 537 cm-1)和糖类(1 069,1 054 cm-1)具有明显的红外指纹特征。螺旋藻粉中的主要成分为蛋白质和糖类,主要辅料为糊精。比较28个不同厂家螺旋藻粉的红外指纹图谱,计算图谱相关系数确定出辅料添加比例的高低。建立吸收峰强度比和蛋白质含量的关联标准曲线,形成依据红外光谱测定样品蛋白含量的方法,与凯氏定氮法测定结果相对偏差小于5%,为螺旋藻粉品质鉴定提供了一种简便、快速、无损的新方法。     

Growth,thermal and optical properties of cis-2,6-diphenyl-3-isopropylpiperidin-4-one – A new class of organic NLO material

A new class of organic nonlinear optical crystalline material, cis-2,6-diphenyl-3-isopropylpiperidine-4-one (3IPO), was prepared. The single crystals of the title material with good optical quality have been grown from its benzene solution by slow evaporation solution growth technique at ambient temperature. Vickers micro hardness measurement studies showed that the crystal belongs to a softer material category. The grown crystals were characterized through the spectroscopic techniques such as PXRD, UV–visible, FTIR and ¹H NMR spectra. The powder XRD reveals the structure of the crystal to be monoclinic system. The UV–visible spectrum was recorded to find the suitability of the title crystal for optical applications. FTIR & ¹H NMR spectra were recorded to confirm the presence of various functional groups and the molecular structure, respectively. The thermal stability of the crystal was established by TGA/DTA analysis. The second harmonic generation (SHG) in the crystal was confirmed using the modified Kurtz–Perry powder test employing Nd:YAG laser as the source of IR radiation and the SHG efficiency was found to be closer that of standard KDP.