Alkalimetric Determination of the Acid Number of Oils and Fats in Surfactant-Stabilized Emulsions

It was shown that the acid number of oils and fats emulsified in aqueous solutions of surfactants can be determined by alkalimetry. Effective pK values of pure long-chain carboxylic acids and acids from some edible oils were determined in different surfactant emulsions. Effective pT values were found for some acid–base indicators in an emulsion stabilized with a mixture of dodecylpyridinium chloride and Triton X-100. Conditions were selected for the determination of the acid number of oils and fats in emulsions based on a mixture of cationic and nonionic surfactants by alkalimetry with the detection of the titration end-point by pH-metry and with the Cresol Red indicator.     

快速测定磷酸氢钙中磷

磷酸氢钙作为一种添加剂广泛应用于食品、饲料等行业,而磷酸氢钙中磷含量的控制非常重要。测定磷含量的方法有比色法、容量法、重量法等。比色法大多适用于低磷样品,容量法适用范围小。磷酸氢钙中磷含量的标准测定方法是采用磷钼酸喹啉重量法,但该方法操作繁琐,而喹钼柠酮试剂不太稳定,需避光保存。有人对滴定法进行改进,提出直接用碱滴定磷酸盐中磷含量,尽管该方法操作简单快速,但用来测定磷酸氢钙中的磷含量时,结果严重偏高。     

高效液相色谱法测定人血清中阿西美辛和吲哚美辛

摘要：建立了测定人血清中阿西美辛及其活性代谢物吲哚美辛的高效液相色谱法。分析柱为Spherisorb-C8（5μm）,4.6mm×250mm,流动相为V（醋酸盐缓冲液,pH4.6）:V（乙腈）:V（甲醇）=55:40:5,流速1.0mL/min,检测波长254nm。血清中药物质量浓度为12.5μg/L～1.6mg/L时,阿西美辛、吲哚美辛峰高与内标甲苯磺丁脲峰高比值和质量浓度呈良好的线性关系;阿西美辛日内、日间变异系数分别为3.6％和5.6％,平均回收率为78.3％;吲哚美辛日内、日间变异系数分别为2.4     

Alkalimetric determination of mercaptans through trithiocarbonic acid formation

A simple and rapid alkalimetric method for the determination of mercaptans through trithiocarbonic acid formation is described. The mercaptans are titrated in tert.-butanol in the presence of carbon disulphide with standard aqueous sodium hydroxide, with phenolphthalein as indicator. The -SH group is smoothly, rapidly and quantitatively transformed into the group under the specified conditions. The method has been extended to the analysis of mercaptan-carboxylic acid and mercaptan-trithiocarbonate mixtures.     

Alkalimetric determination of amoxycillin trihydrate in non-aqueous medium

A simple method for determination of amoxycillin by non-aqueous titration in dimethylformamide medium is described. The relative standard deviation is 0.3%.     

Determination of Rutin in Plant Extracts and Emulsions by HPLC-MS

A method for the determination of rutin was developed from in an O/W emulsion with decyl oleate and Ceteareth-20 containing Ginkgo biloba L., Hedera helix L., and Thymus vulgaris L. extracts. Total quantification of rutin was performed by determination in the aqueous and oily phase. Rutin was extracted from the oily phase by ultrasonication for 30 min at 37°C in methanol and resolved by liquid chromatography on a column containing a Gemini 3 µ C18 110A stationary phase.

Chromatography was carried out using gradient elution with the mobile phase composed of water:formic acid and water:acetonitrile:formic acid, which was varied from 100:0.1 to 50:50:0.1 (v/v/v) over 80 min and delivered at a flow rate of 0.3 ml/min. The analytes were quantified using a UV-VIS absorption spectrometer at a wavelength of 254 nm and a single quadrupole mass spectrometer employing an ESI interface operated in the positive ion mode with single ion monitoring at m/z = 609.14.

Finally, a simple and rapid method for the extraction and determination of rutin in hydrophilic and lipophilic phases of an O/W emulsion with good precision and acceptable recovery was developed. This method might be of special importance for the analysis of rutin and other flavonoids in O/W or W/O emulsion matrices.     

利用偶联反应光度法测定羟胺体系的研究及应用

利用羟胺与碘反应生成亚硝酸 ,然后与对氨基苯磺酸发生重氮化反应 ,再与 α-萘胺偶联形成偶氮化合物 ,从而建立了测定羟胺的新光度法。方法线性范围为 2 .0× 1 0 - 6 ～1 .5× 1 0 - 5mol/L ,表观摩尔吸光系数为 3.1× 1 0 4 L· mol- 1· cm- 1,应用于水中羟胺和试剂丁二酮肟含量的测定 ,结果满意。     

Colorimetric Sensing of Nitroaromatic Energetic Materials Using Surfactant-Stabilized and Dithiocarbamate-Functionalized Gold Nanoparticles

Abstract

There is an increasing need for sensitive/selective determination of explosive traces in soil and post-blast debris for environmental and criminal investigations. A colorimetric sensor was developed to detect and quantify trinitrotoluene (TNT) and tetryl by the use of surfactant-stabilized and dithiocarbamate-functionalized gold nanoparticles (AuNPs). The sensor was manufactured by modifying the nanoparticles with the cationic surfactant cetyl trimethyl ammonium bromide and incorporating diethyldithiocarbamate (DDTC) in the AuNPs synthesis. DDTC firmly bound to AuNPs may show charge-transfer interactions with the —NO₂ groups of the analytes, and a color change proportional to analyte concentration accompanied the agglomeration of nanoparticles, at which the absorbances were recorded at 534?nm and 458?nm for TNT and tetryl, respectively. Although the limit of detection was 8?mgL^?1 (3.52?×?10^?5?molL^?1) for TNT and 0.8?mgL^?1 (2.78?×?10^?6?molL^?1) for tetryl, providing moderate sensitivity, the cost was greatly reduced compared to those of other thiol-functionalized AuNPs sensors. Possible interferences of other energetic substances in synthetic mixtures, of camouflage materials used in passenger belongings (e.g., detergent, sugar, caffeine, and paracetamol) and common soil ions were also examined. The method was statistically validated against a reference gas chromatography/mass spectrometry method. This sensor may pave the way for the manufacture of novel low-cost nitroaromatic explosive sensors made of DDTC-based pesticides.     

利用偶联反应光度法测定羟胺体系的研究及其应用

利用羟胺与碘反应生成亚硝酸,然后与对氨基苯磺酸发生重氮化反应,再与α-萘胺偶联形成偶氮化合物,从而建立了测定羟胺的新光度法.方法线性范围为2.0×10-6～1.5×10-5 mol/L,表观摩尔吸光系数为3.1×104 L.mol-1.cm-1,应用于水中羟胺和试剂丁二酮肟含量的测定,结果满意.     

Use of Catecholoxygenase for Determination of Catechol

Abstract

A cell extract from Trichosporon cutaneum containing catechol 1,2-oxygenase catalyzes the oxidation of catechol to cis,cis-muconic acid. The absorbance of the cis,cis-muconic acid at 260 nm can be correlated with the initial catechol concentration in the range 5 × 10^?6 M to 5 × 10^?5 M in aqueous solutions. This enzymatic assay has been applied to the determination of catechol in aqueous samples derived from coal processing.     

Conformation and Atropisomeric Properties of Indometacin Derivatives

The stereochemistry around the N‐benzoylated indole moiety of indometacin was studied by restricting the rotation about the N? C7′ and/or C7′? C1′ bond. In the 2′,6′‐disubstituted ones, an atropisomeric property was found and the atropoisomers were separated and isolated as stable forms. Their biological abilities to inhibit cyclooxygenase‐1 (COX‐1) and cyclooxygenase‐2 (COX‐2) were examined. Only the aR‐isomer showed specific inhibition of COX‐1, and COX‐2 was not inhibited by either atropisomer. Conformational analysis in NMR studies and X‐ray crystallography, and CD spectra in combination with calculations were utilized to elucidate the bioactive conformations.     

用溶氧仪代替滴定法测定BOD5中DO

BOD5是指水样经中和及去除毒性物质或经稀释后 ,置于培养瓶中 ,在 2 0℃暗处放置五天 ,由测定最初及五天后溶解氧 ,得出五天内的耗氧量 ,再根据稀释倍数求得。BOD5是根据水中有机物耗氧量的多少间接表示出水中有机物的量 ,是一种间接表示水体受有机物污染程度的指标 ,是水质监测中的重要项目之一[1] 。在BOD5测定中对溶解氧的测定一般使用滴定法 ,此方法要配制MnSO4 等多种试剂 ,并定时标定Na2 S2 O3标准溶液 ,本法使用溶氧仪代替滴定法直接测定溶解氧 ,不需要配制试剂及标定标准溶液 ,方法简单、操作快捷 ,不但符合葡萄糖 谷氨酸试…     

Alkalimetric determination of hydrophobic pharmaceuticals using stabilized o/w emulsions

Protolytic properties of (+)-(S)-2-(6-methoxynaphthalen-2-yl)propanoic acid (naproxen), 2-(3-benzoylphenyl)propionic acid (ketoprofen), 4-chloro-N-(2-furylmethyl)-5-sulfamoylanthranilic acid (furosemide), and N-(2,3-dimethylphenyl)anthranilic acid (mefenamic acid) in “oil-in-water” emulsions stabilized by surfactants were studied. The procedures for alkalimetric determination of naproxen, ketoprofen, furosemide, and mefenamic acid in emulsion media with indication of the equivalence point pH-metrically and with the use of indicators were proposed.     

Use of Nitric Acid for Determination of Lignosulfonates

The possibility of using the reaction of nitric acid with lignosulfonates for their quantitative determination in aqueous solutions was studied.     

Encapsulation of Flavors in Emulsions for Beverages

Though stable in dilute form for very long periods of time, simple mono-emulsifier flavor emulsions based on gum acacia or modified starch are fairly limited in their ability to provide functionality beyond simple dispersion. This review highlights many of the enhancements on traditional emulsions, ranging from new materials to novel combinations of materials and processes. The development of more sophisticated dispersion technologies employing complex mixtures of biopolymers as well as low molecular weight surfactants, and novel multilayered interfacial structures, is on an intersecting course with a growing need for enhanced emulsion functionality in beverages, such as controlled release, protection, taste masking, and targeted delivery. Novel raw materials, molecular assemblies, processes and applications are discussed in this review.     

Determination of the Phase Inversion Temperature of Orange Oil/Water Emulsions by Rheology and Microcalorimetry

Abstract

In low-energy emulsification processes, phase inversion occurs when the phases of a dispersion exchange, because of changes in the medium's properties. This paper reports experiments to determine the phase inversion temperature (PIT) of orange oil/water emulsions stabilized by nonionic surfactants. Two techniques were employed: rheology, which is already commonly used to obtain the PIT, and microcalorimetry, which has been proposed as a new technique. Continuous monitoring of the emulsions' viscosity permitted identifying different phenomena that occur while the temperature varies. For all the dispersions prepared, the rheological curves obtained showed two peaks, one attributed to the phase separation process and the other to the phase inversion phenomenon. The microcalorimetry technique showed two endothermic transitions as the dispersion's temperature increased. The initial temperatures were comparable to those obtained by rheology. The influence of the surfactant concentration and the hydrophilic-lipophilic balance (HLB) of the mixture of surfactants and the reduction in volume of the phases at the phase inversion temperature were also evaluated. In general, both methods used to evaluate the phase inversion of the orange oil/water systems (rheology and microcalorimetry) presented concordant results, both for the phase separation process and the phase inversion temperature.     

Thermoset Alkyd-Acrylic Hybrid Emulsions for Coatings

Alkyd acrylic hybrid emulsions can offer cost/performance advantages over common 1K coatings such as polyurethane dispersions (PUDs), acrylic emulsions and blends. Hybrid emulsions with different ratios of alkyd resin to acrylic monomers were synthesized. Emulsion with resin-to monomer ratio of 1:1 (wt/wt) with total solids as high as 50% had a shelf stability of more than 8 months. Morphology of hybrid emulsions was studied by scanning electron microscopy. Hybrid emulsions were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis. Films obtained from the hybrid emulsions were found to be homogeneous and exhibited excellent thermal and coating properties.     

Protein-Polysaccharide Interactions for Stabilization of Food Emulsions

Proteins, polysaccharides and their blends, as examples of natural biopolymers, are surface active materials. Biopolymers may be considered as amphiphilic macromolecules that play an essential role in stabilizing food formulations (foams, emulsions and dispersions). Under specific conditions (such as protein-to-polysaccharide ratio, pH, ionic strength, temperature, mixing processing), it has been stated that proteins and polysaccharides form hybrids (complexes) with enhanced functional properties in comparison to the proteins and polysaccharides alone. Different protein-polysaccharide pairs are reviewed with particular attention to the emulsification capability of their mixtures. In the case of uncomplexed blends of biopolymers, competitive adsorption onto hydrophobic surfaces is generally reported. Conversely, electrostatic complexation between oppositely charged proteins and polysaccharides allows better anchoring of the new-formed macro-molecular amphiphile onto oil-water interfaces. Moreover, improved thermal stability and increased resistance to external treatment (high pressure) involved in food processing are obtained. This review presents basic and applied knowledge on protein-polysaccharide interactions in aqueous medium and at the oil-water interface in food emulsion systems. Electrostatic interactions and thermodynamic incompatibility in mixed biopolymer solutions are correlated to the functional properties (rheology, surface hydrophobiciry, emulsification power) of these interesting blends. Basic and industrial selected systems of different families of hydrocolloids (as gum Arabic, galactomannans, pectins) and protein (caseins, whey, soya, gelatin) mixtures are reviewed.     

On the Viscosity of Dilute Emulsions

The slow motion of a liquid droplet in a shear flow in the presence of surfactants is studied. The effects of the interfacial viscosity, Gibbs elasticity, surface diffusion and bulk diffusion of surfactants in both phases are taken into account. The analytical solution of the problem for small Reynolds and Peclet numbers gives a simple criterion for estimation of the tangential mobility of the droplet interface. By applying the standard procedure for averaging of the stress tensor flux at an arbitrary surface of the dilute emulsion, an analytical formula for the viscosity of emulsions in the presence of surfactants is derived. The result is a natural generalization of the well-known formula of Einstein for the viscosity of monodisperse dilute suspensions and of the expressions derived by Taylor and Oldroyd for the viscosity of monodisperse dilute emulsions taking into account the Marangoni effect. Copyright 2001 Academic Press.     

Viscosity-Concentration Equation for Emulsions of Nearly Spherical Droplets

A new modified form of the equation of N. Phan-Thien and D. C. Pham (J. Non-Newtonian Fluid Mech. 72, 305 (1997)) is proposed to describe the viscosity-concentration behavior of emulsions of nearly spherical droplets. The proposed equation, as well as other existing theoretical equations, is evaluated in light of a large body of experimental data on concentrated emulsions, covering a broad range of dispersed-phase to continuous-phase viscosity ratios (4.15x10(-3) to 1.17x10(3)). In general, the experimental data exhibit large deviations from the existing theoretical equations; for example, the theoretical equation of Phan-Thien and Pham underpredicts the relative viscosity of concentrated emulsions by a large amount. The equation proposed in this work describes the experimental viscosity data of different emulsion systems remarkably well. Copyright 2000 Academic Press.