比值光谱—导数分光光度法同时测定纤维上的二组分混合染料

研究了用比值光谱－导数分光光度法同时测定两组分混合染料体系中分散大红ＢＷＦＬ和分散红玉ＺＧＦＬ的方法。回收率在９５．６％～１０７．５％。方法已用于分析纺织纤维上分散大红和分散红玉二元混染体系。     

Fe2O3超微粒／硬脂酸得合LB膜的制备和表征研究

用超声分散的方法将Ｆｅ２Ｏ３超微粒分散于硬脂酯／正己烷／氯仿溶液中，用ＬＢ膜技术进行组装。结果表明：ＦｅＯ３超微粒能均匀地分散在有机溶剂中，并且能够被硬脂酸包裹；Ｆｅ２Ｏ３超微粒／硬酯酸单分子膜的成膜性能良好，Ｆｅ２Ｏ３超微粒／硬脂酸复合ＬＢ膜具有层状结构；在Ｆｅ２Ｏ３超微粒的晶格结构和硬脂酸单分子膜的晶格结构相匹配的情况下，Ｆｅ２Ｏ３超微粒能够被有序组装。     

用系数倍率法测定染料分散灰N中的三组份含量

分散灰 N(简称灰 N)主要是由分散蓝2BLN,分散红3B,分散黄 RGFL(分别简称为分蓝,分红,分黄)三种染料组成的。本文采用紫外-可见光谱系数倍率法直接测定灰 N 中的三个组分的百分含量。1.确定测定波长和 K 值:称取分蓝0.0124g,分红0.0135g,分黄0.0200g,用 N,N-二甲基甲酰胺(DMF):水=1:1为溶剂,分别配制浓度在2.4～24mg/L;2.7～27mg/L,4～40mg/L 范围内的分蓝、分红、分黄一系列标准液,取三种溶液中一种溶液,用 UV-250分光光度计测定三者在700～300nm 处的 UV-     

Fe_2O_3超微粒/硬脂酸复合LB膜的制备和表征研究

用超声分散的方法将Ｆｅ２Ｏ３超微粒分散于硬脂酸／正己烷／氯仿溶液中，用ＬＢ膜技术进行组装。结果表明：Ｆｅ２Ｏ３超微粒能均匀地分散在有机溶剂中，并且能够被硬脂酸包裹；Ｆｅ２Ｏ３超微粒／硬酯酸单分子膜的成膜性能良好，Ｆｅ２Ｏ３超微粒／硬脂酸复合ＬＢ膜具有层状结构；在Ｆｅ２Ｏ３超微粒的晶格结构和硬脂酸单分子膜的晶格结构相匹配的情况下，Ｆｅ２Ｏ３超微粒能够被有序组装。     

流动注射分析中试样分散的对流—扩散理论

用两种方法求解适合于单一平直管道且无化学反应的流动注射分析（ＦＩＡ）体系的对流－扩散方程，得到了述塞状进样在管道中分散后的浓度分布公式，从而得到Ｆ曲线，讨论了反应管和采样管的内径和长度、流速和扩散系数对峰形和分散度的影响；采用数值法解出半峰宽和扩散系数的关系，提出了两种测定扩散系数的方法，为ＦＩＡ体系的设计和指示物质、操作条件的选择提供了理论依据。     

含有二色性染料的PDLC的光电性能

用聚合分相法,在Ｅ－７液晶中掺入二色性液晶分散蓝,制成聚合物分散液晶膜。测定了它的光电性能。与不加二色性染料的聚合物分散液晶膜比较,膜对比度提高,响应时间τｏｎ保持不变,松驰时间τｏｆｆ略有增加。     

带羧基单分散彩色微球的制备

采用两步活性溶胀种子聚合法, 制备了可用于免疫检测的3种不同颜色的表面带有羧基功能基的粒径在400—800 nm之间的彩色单分散微球. 先用无皂乳液聚合法制备出单分散聚苯乙烯种子, 然后用邻苯二甲酸二正丁酯(DBP)作为溶胀剂对微球进行溶胀, 溶涨后的种子模板再用混溶的苯乙烯、二乙烯苯、丙烯酸、双键彩色染料以及引发剂(BPO)溶胀, 升温聚合后得到理想的单分散微球. 考察了DBP和单体用量、各单体配比及染料对微球的形貌和单分散性的影响.     

液相色谱-串联质谱测定纺织品中分散黄23和分散橙149

建立了高效液相色谱法(HPLC)和液相色谱-串联质谱法(LC-MS/MS)测定纺织品中分散黄23和分散橙149含量的方法.样品上的分散染料经氯苯蒸汽完全剥离纤维,浓缩后的残留物用甲醇定容,以0.1% H3PO4(或0.1%甲酸)和乙腈为流动相,经反相色谱柱分离后,用二极管阵列检测器(DAD)在420 nm处测定,并用电喷雾串联质谱确认.分散黄23和分散橙149的定量离子对分别为m/z 303/105和m/z 459/399.分散黄23和分散橙149的检出限(S/N=3):HPLC法为2.0和1.0 mg/kg,LC-MS/MS法都为1.0 μg/kg.HPLC在0.5～250 mg/L、LC-MS/MS在0.5～200 μg/L范围内,线性相关系数都大于0.995.方法的回收率在92.1%～98.7%之间,批间RSD都小于8.0%,含有分散黄23的阳性样品重复测试的RSD也小于8.0%.     

易潮解化合物AlCl3和FeCl3在载体表面的分散状态及分散量

易潮解化合物ＡｌＣｌ３和ＦｅＣｌ３在载体表面的分散状态及分散量宗越潘晓民段连运＊谢有畅（北京大学物理化学研究所，北京１００８７１）关键词氯化铝，氯化铁，氧化铝，分散状态，分散阈值，Ｘ射线衍射无水ＡｌＣｌ３和无水ＦｅＣｌ３同属Ｌ酸，在酸催化中起着重要的...     

氧化铁在ZnO上分散的结构状态及其表征

采用（ＮＨ_４）_３［Ｆｅ（Ｃ_２Ｏ_４）_３］·ｘＨ_２Ｏ的水溶液含浸，Ｆｅ（ＮＯ_３）_３．９Ｈ_２Ｏ水溶液饱和浸渍（含浸）以及Ｆｅ（ＡｃＡｃ）_３的甲苯溶液热吸附三种方法制备了在ＺｎＯ上分散的氧化铁体系。用多种物理化学手段对用不同方法制备的分散体系进行了细致的表征，氧化铁在ＺｎＯ上形成单层分散是困难的。Ｆｅ~（３＋）一般进入到ＺｎＯ载体的表层，结构环境类似于ＺｎＦｅ_２Ｏ_４微晶中的Ｆｅ~（３＋），分散的Ｆｅ~（３＋）通常处于高自旋态，配位对称性并不是正交畸变。在ＺｎＯ上形成尖晶石的趋势最强。在亚单层铁含量范围内，通常形成表面ＺｎｘＦｅ_ｙＯ_ｚ。当铁含量超过单层阈值时，既生成ＺｎＦｅ_２Ｏ_４簇也有ＦｅＯ_ｘ簇存在。无论是ＦｅＯ_ｘ或ＺｎＦｅ_２Ｏ４簇还是表面的Ｚｎ_ｘＦｅ_ｙＯｚ，其Ｆｅ_（３＋）在实验温度范围内，很难被还原为零价铁，ＦｅＯ_ｘ较之Ｚｎ_ｘＦｅ_ｙＯ_ｚ物种难以还原且比体相ａ－Ｆｅ_２Ｏ_３中Ｆｅ~（３＋）要难还原得多。由热吸附法制得的ＦｅＯ_ｘ和ＺｎＦｅ_２Ｏ_４簇具有很低的催化活性，而由含浸法制得的表面Ｚｎ_ｘＦｅ_ｙＯｚ的反应性能有明显的改善。ＺｎＯ载体上不同含铁物种的反应性由Ｆｅ~（３＋）的还原性及是否存在活泼     

Measurement and correlation of solubilities of C.I. Disperse Red 73, C.I. Disperse Yellow 119 and their mixture in supercritical carbon dioxide

The solubilities of disperse dyes and their mixture in supercritical carbon dioxide are important to the fundamental research and development of supercritical fluid dyeing (SFD). The solubilities of Disperse Red 73, Disperse Yellow 119 and their mixture in supercritical carbon dioxide were measured in the temperature range from 343 to 383 K and pressures from 12 to 28 MPa by a static-recirculation method. The results show that over the entire range of experimental conditions in the binary (Disperse Red 73 + CO₂ and Disperse Yellow 119 + CO₂) and ternary (Disperse Red 73 + Disperse Yellow 119 + CO₂) systems, the solubilities increased with increasing pressure and temperature and were clearly affected by the molecular polarity of the dyes. A co-solvent effect and a competing dissolution effect existing in the ternary system led to the increase and decrease in the solubilities of Disperse Yellow 119 and Disperse Red 73, respectively. The solubility data of the two dyes and their mixture were correlated with two empirical models—the Chrastil and the Mendez-Santiago/Teja (MT) model.     

阳离子膨润土对分散染料的吸附动力学研究

研究了阳离子膨润土(EPI-DMA/Bt, PD/Bt, CTMAB/Bt)对分散染料(分散黄棕S-2RFL, 分散大红S-R, 分散蓝SBL, 分散黄SE-6GFL)的吸附动力学行为. 结果表明, 阳离子膨润土对分散染料的吸附过程符合二阶段吸附速率方程, 各阶段具有不同的吸附动力学常数(k1, k2)以及吸附活化能(Ea1, Ea2)、活化焓(ΔH*1, ΔH*2)和活化熵(ΔS*1, ΔS*2); 在阳离子膨润土对分散染料的吸附过程中, k1随着阳离子插层剂烷烃链的增加而增大, 表明较大的晶片层间距, 疏水的层间域和表面正电荷增加均有利于吸附速率增大; 对于两个吸附动力学阶段, ΔH★1<-TavΔS★1, △H★2<-TavΔS★2和ΔG★>0表明整个吸附过程活化熵的影响大于活化焓.     

Silicone nanomicelle dyeing method on polyester fibre: Comparative evaluation of chemical properties,fastness properties,and DFT

Disperse Red 177(9a), Disperse Red 343(9b), Disperse Blue 165(9c), Disperse Blue 165.1(9d), Disperse Blue 366(9e), and Disperse Blue 148(9f) were examined in the solvent. During silicon nanomicelle dyeing, we employed 9(a–f) azo disperse dyes on polyester. On polyester fabric, dye 9(a–f) offers equal washing, light, and rubbing fastness in both the conventional and silicone nanomicelle techniques. The dye can now be transported directly into the fibre core without the use of auxiliary dyes owing to the reduction in the particle size of azo dyes, which is made possible by nanoemulsions superior dispersion. The levelling property of the dispersed dye is enhanced by the dyeing process. When both techniques are applied, the lightfastness properties of all dyes are improved. It provides a very good to outstanding protection factor for textile materials. These 9(a–f) azo disperse dyes have moderate to outstanding photostability, net electrophilicity index, and lightfastness.     

Stability of Dye Dispersions in the Presence of Various Surface Active Agents and Additives

Disperse dyes are hardly soluble in water. They are usually milled in the presence of large amounts of dispersing agents in the dye industry. The type and amount of these materials can affect the disperse ability of dyes in aqueous media. In this article, stability of prepared dye dispersions in the presence of various surface active agents and additives were investigated. In this respect, various dispersing agents such as Irgasol DAM, Asutol 644, Dispertane MF, and Irgasol P800 were used to prepare dye dispersions in milling stage. Furthermore, the formulations of dye dispersions were obtained by adding β-cyclodextrin, urea, and wetting agent. The dye dispersion quality was determined by its filtering property, turbidity, and centrifuging method. The obtained results proved the stability of dispersion containing of Irgasol DAM, wetting agent, and β-cyclodextrin as dispersing auxiliaries in dyeing process of disperse dye on polyester fabrics in high temperature method was the highest as compared to other dispersions. From the experimental results, it was found out that stability of prepared dispersions was improved by the presence of β-cyclodextrin. Also, utilization of β-cyclodextrin in formulations of dye dispersions caused to increasing of stability of dispersion in the dyeing of polyester fabrics.     

高效液相色谱-电喷雾串联质谱法快速分离鉴定纺织品中的9种致癌染料

采用高效液相色谱-电喷雾串联四极杆质谱(HPLC-ESI-MS/MS)在选择反应监测(SRM)模式下分离鉴定纺织品中禁用的9种致癌染料。用甲醇超声同时提取天然纤维和化学纤维上的染料,以5 mmol/L乙酸铵和乙腈为流动相在C18柱上于前段洗脱酸性红26、直接蓝6、直接黑38和直接红28(采用电喷雾质谱负离子模式检测),于后段洗脱碱性红9、碱性紫14、分散蓝1、分散橙11和分散黄3(采用电喷雾质谱正离子模式检测),实现了对不同种类纤维织品中分属4类性质不同染料的一次提取和一次分析检测。通过比较试样与标样的色谱保留时间和质谱图中子离子的相对丰度比,可准确鉴别纺织品中的致癌染料。     

Synthesis of some novel heterocyclic dyes derived from pyrazole derivatives

Diazotized aryl amines were coupled with 3-substituted 5-amino pyrazoles to produce a series of novel 3-substituted 5-amino-4-arylazopyrazoles. Also, 3-substituted 5-amino-pyrazoles were diazotized and coupled with different phenols to give the corresponding novel 3-substituted 5-aryl azo pyrazoles. These dyes were characterized by elemental analysis and spectral data, applied to different types of fibres (wool, polyester and a blend of wool/polyester as disperse dyes) and their fastness properties were evaluated.     

Fast throughput, highly sensitive determination of allergenic disperse dyes in textile products by use of sample composition

A simple, highly sensitive and fast procedure for the control of allergenic disperse dyes in textile products was optimized. The method is based on ultrasound assisted extraction of textile samples with 20 mL of methanol under controlled conditions (15 min, 70 °C) followed by separation and analysis by LC-MS-MS. The sample preparation process was optimized by means of a surface response experimental design and provided quantitative recoveries of dyes, much better than the poor recoveries provided by current standard procedures. The chromatographic separation was optimized by means of computer-assisted method development by use of a special chemometric tool developed specifically for LC-MS systems, as previously reported by the authors. The result is a rapid chromatographic procedure that enables accurate quantification, at very low concentrations, of all 23 allergenic and/or carcinogenic disperse dyes considered. Matrix effects in the LC-MS procedure were studied. Under the experimental conditions, both conventional and strategic sample composition are proposed as efficient procedures that reduce the costs and work involved in the control of allergenic dyes in finished textile products. The benefits of strategic sample composition are demonstrated by means of an example case study, and the pros and cons of preparing the composite samples from sample extracts or directly from textile products are discussed.     

Removal of Disperse Dyes from Water Using Surfactant Treated Alumina

An alumina surface was modified by adsorption of an anionic surfactant, sodium dodecyl sulfate (SDS). Typical S‐shaped isotherm of surfactant on alumina was observed. The adsorption of Disperse Red‐11, Disperse Blue‐26 and Disperse Red‐156 on alumina and surfactant treated alumina has been investigated. The enhancement in adsorption of these disperse dyes on surfactant treated alumina is observed, which may be attributed to their solubilization in surfactant aggregates formed at the solid/liquid interface. The effect of pH on adsorption has been studied. The adsorption is greatly influenced by pH of the medium. The applicability of the Langmuir model and the Dual‐Mode sorption model (DSM) were tested for equilibrium data.     

高效液相色谱-线性离子阱/静电场轨道阱质谱快速筛查确证生态纺织品中22种致敏性分散染料

建立了基于高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(HPLC-LTQ/Orbitrap MS)快速筛查确证生态纺织品中22种禁用分散染料的分析方法。样品在95 ℃水浴条件下经吡啶/水(1:1, v/v)振荡提取后,以CAPCELL PAK C₁₈色谱柱分离,以乙腈和5 mmol/L乙酸铵(含体积分数为0.01%的甲酸)作为色谱流动相进行梯度洗脱,采用正、负电喷雾(ESI)离子化模式,利用一级母离子的精确质量数和保留时间对22种分散染料进行快速筛查,利用碰撞诱导解离(CID)下得到的二级碎片离子进行确证。22种分散染料在各自浓度范围内线性关系良好(r²> 0.99),方法的定量限(LOQ)为0.125~2.5 mg/kg。除分散黄49外,绝大多数染料在涤纶布、棉涤混纺布两种纺织品基质中的加标回收率在65%~120%之间,相对标准偏差小于15%。应用本方法对涉及多种纤维类型的40余件纺织品样品进行了筛查,其中一个样品检出分散橙37/76。该方法简便、快速,其选择性高,抗干扰性能好,结果准确可靠,可用于纺织品中分散染料的检测。     

Synthesis and crystal structures of two hetarylazo indole disperse dyes

Two new heterocyclic monoazo disperse dyes were prepared by diazotizing 2-amino-5-methylthiazole and ethyl-1-(2-aminothiazol-4-yl)acetate and coupling with 1,2-dimethyl-indole. Characterization of the dyes was carried out by using UV–vis, FTIR, ¹H-NMR and MS spectroscopic techniques. The structures of the dyes have been determined by single-crystal X-ray diffraction method. The maximum absorption peaks (λ_max) in the ultraviolet and visible (UV–vis) spectra of the hetarylazoindole dyes have been determined by using the density-functional (DFT method) and time-dependent density-functional (TD-DFT method) theories. Excellent agreement was found between the calculated and experimental λ_max values.