Determination of fatty alcohols in fatty alcohol sulfates

A simplified procedure for the quantitative determination of very small amts of fatty alcohols in fatty alcohol sulfates has been developed. In the present work this procedure was applied to the determination of lauryl alcohol in lauryl alcohol sulfate.     

2,4-二磺酸基苯甲醛含量的测定

本文介绍了一种测定2,4-二磺酸基苯甲醛含量的方法.2,4-二磺酸基苯甲醛与亚硫酸氢钠加成反应生成4-(羟基磺酸基甲基)苯-1,3-二磺酸,再与碳酸氢钠共热释放出亚硫酸氢钠,然后用碘量法测亚硫酸氢钠含量,从而分析2,4-二磺酸基苯甲醛的含量.     

1，3一二氨基胍盐酸盐的高效液相色谱分析

提出用高效液相色谱法测定1,3-二氨基胍盐酸盐的含量,选用甲醇与乙酸铵缓冲盐体积比75：25为流动相,c8色谱柱,检测波长314nm。试验结果表明：测试结果的相对标准偏差小于2．03％;回收率在97．8％～100．2％;1,3-二氨基胍盐酸盐和三氨基胍盐酸盐得到较好的分离。该法操作简单、实用且定量分析结果准确稳定。     

Alcohol ether sulfates in shampoos

Mono-, di- and triethanolamine sulfates of several different molecular weight alcohol ether sulfates were formulated into shampoos. The ethylene oxide content of the alcohol ethoxylates varied from about 20 to 60%, although 40% was usual. The shampoo formulation was 20% active ether sulfate and 5% foam stabilizer. Lauric diethanolamide and amine oxides were used as foam stabilizers. The shampoos were tested for quality and quantity of foam, viscosity and cloud point. Although no “hair effects” tests were run, a limited home use test was made. Alcohol ether sulfate shampoos are equal or superior to several popular commercial products on the basis of a laboratory foam test. They are comparable in foam to alcohol sulfates in similar formulations. Cloud points of these shampoos were generally good. Amine oxide foam stabilizers reduced the cloud point more than the amide. Viscosities of the shampoos were readily controllable. Although the choice of alkanolamine, alcohol molecular weight and degree of ethoxylation had some effect on these properties, none were highly critical; this allows considerable leeway in their selection. The home use tests assured us that these shampoos were not obviously deficient in the desired “hair effect” properties. The literature records that alcohol ether sulfates are preferred to alcohol sulfates for low skin and eye irritation. By varying the free oil (unsulfated ethoxylate) content and making the proper choice of ether sulfate and foam stabilizer, bright and clear liquid shampoos with viscosities from about 10 centipoise to over 50,000 centipoise were made. The latter are essentially gels. Paste shampoos were also made from these ether sulfates. Presented at the AOCS Meeting, Chicago, October 1967. Now with Stepan Chemical Company, Northfield, Illinois.     

化妆品中1，3-二羟甲基-5，5-二甲基海因含量的测定

运用凯氏定氮的原理,采用Turbotherm红外快速模块式消化器及Gerhardt凯氏定氮仪对应用于化妆品中的防腐剂1,3-二羟甲基-5,5-二甲基海因(DMDMH)的量进行测定,得出了较佳消化条件:催化剂3.5 g,浓硫酸8 mL(相对于1 g DMDMH),只需消化80 min;较佳蒸馏时间为5 min。结果表明,试样测定的相对标准偏差(RSD)为0.12%(n=9)。     

Synthesis and surface properties of chemodegradable anionic surfactants: Sodium (2-n-alkyl-1,3-dioxan-5-yl)sulfates

In the reaction of cis- and trans-2-n-alky-5-hydroxyl-1,3-dioxane mixtures with SO₃ · pyridine complex, followed by neutralization with sodium hydroxide or sodium carbonate, a new group of anionic surfactants, i.e., sodium cis- and trans-(2-n-alkyl-1,3-dioxan-5-yl)sulfates were obtained. The hydrophobic intermediates used in the sulfation reaction were obtained in high yields from four-component glycerol acetals by the process of transacetalization and selective crystallization of 1,3-dioxane derivatives. The physical data of the new compounds and some of their surface properties, such as critical micelle concentration (CMC), effectiveness of water surface tension reduction π_CMC, standard free energies of adsorption and micellization, ΔG _ads ^o and ΔG _CMC ^o , surface excess concentration, Γ_CMC, and the surface area demand per molecule, A_CMC, were determined. It was shown that the surface activity of the standard anionic surfactant sodium dodecyl sulfate should be similar to the surface activity of sodium (2-n-decyl-1,3-dioxan-5-yl)sulfate. Part XXX in the series: Chemical Structure and Surface Activity. Part XXIX: Sokołowski, A., B. Burczyk, and H.-R. Holzbauer, Adsorption of n-butyloligooxypropylene-pentaoxyethylene block copolymers at the aqueous solution-air interface, Collid Surfaces, in press.     

卡尔费休容量法测定1,3-环己二酮水分

目的:建立测定1,3-环己二酮水分的方法。方法:运用卡氏容量法测水分。结果:选用醛酮专用试剂,能够准确测定1,3-环己二酮水分。结论:卡尔费休容量法简便,快速、可靠。     

Synthesis and surface properties of chemodegradable anionic surfactants: Diastereomeric (2-n-alkyl-1,3-dioxan-5-yl) sulfates with monovalent counter-ions

Sodium, potassium and ammonium cis- and trans-(2-n-alkyl-1,3-dioxan-5-yl) sulfates 6–8 (alkyl: n-C₉H₁₉, 6a–8a, and n-C₁₁H₂₃, 6b–8b) were synthesized in a reaction of aliphatic aldehydes 1a,b with glycerol 2 followed by separation in high yields of individual geometric isomers of cis-and trans-2-n-alkyl-5-hydroxy-1,3-dioxanes, cis-3a,b and trans-3a,b, followed by sulfation with sulfur trioxide-pyridine complex, and finally neutralization with NaOH, KOH, and NH₄OH, respectively. Physical data of the compounds and some surface properties of 2-n-nonyl derivatives, such as critical micelle concentration (CMC), effectiveness of aqueous surface tension reduction (Π_CMC), surface excess concentration Γ_CMC, and the surface area demand per molecule (A_CMC), were determined. It was shown that the surface activity of these compounds is influenced both by their geometric structure and by the monovalent counter-ion.     

Controlled radical polymerization of conjugated 1,3-dienes with methyl 1,3-butadiene-1-phosphonate

Preparation of new tailor-made phosphorus-containing polydiene materials via controlled radical copolymerization of dimethyl 1,3-butadiene-1-phosphonate (BP^Me) with chloroprene (CP) or isoprene (IP), by using, respectively, AIBN or an alkoxyamine derivative as initiator, is reported. The corresponding materials have been microstructurally characterized by ¹H and ³¹P NMR spectroscopies.     

1,3-2,4-二(3,4-二甲基)亚苄叉山梨醇溶解度的测定

利用基团贡献法计算了聚丙烯成核剂DDMBS的溶解度参数(δ=26.54J1/2.cm-3/2),在此基础上计算了部分溶剂与DDMBS样品的相容性参数,其中P(DDMBS～C6H5CH2OH)=26.94,P(DMDBS～C6H5CH2CH2OH)=35.15,P(DDMBS～1,2-二氧六环)=113.83,即苯甲醇是DDMBS成核剂的最好溶剂,其次是苯乙醇,再次是1,4-二氧六环;利用溶解度参数理论,预测DDMBS的混合溶剂为苯甲醇～甲醇和苯乙醇～甲醇;用浊度滴定法测定了成核剂DDMBS的溶解度参数,测定值为δ实验=25.24(J/ml)1/2,与用基团贡献法计算值基本一致;测定了DDMBS试样在不同溶剂中的溶解度,并建立了该成核剂试样在不同溶剂中的溶解度与温度的关系方程;在相同温度下,DDMBS在苯甲醇中溶解度稍大于在苯乙醇中的溶解度,DDMBS在1,4-二氧六环中的溶解度小于在苯甲醇、苯乙醇中的溶解度。     

卤水中硫酸根的去除方法

根据江西赣中氯碱制造有限公司的工业实践,探讨了卤水中硫酸根的去除方法,证明了冷却法除硫酸根不但可以除净卤水中的SO4^2-,还可以提高卤水的掺用率、降低烧碱的生产成本,是全卤制碱除SO4^2-的一条新途径。     

1H-NMR-Untersuchungen zur innermolekularen Beweglichkeit in substituierten 1,3-Diazabutadienen

¹H-N.M.R. Spectroscopic Investigations on Innermolecular Mobility of Substituted 1,3-Diazabutadienes Two isomerization processes in substituted 1,3-diazabutadienes can be observed by the method of dynamic n.m.r. spectroscopy. From coalescence phenomena the free activation enthalpies ΔG± are determined and discussed with regard to substituent effects and solvent dependency.     

Synthesis and anticoagulant activity of pectin sulfates

In this article, we describe the first use of trisulfonated sodium amine as a sulfating reagent for preparing pectin sulfate in aqueous solution. The main reaction parameters that were expected to affect the degree of substitution (DS) were studied. The optimal reaction conditions for the synthesis of pectin sulfate were found to be as follows: the pH of the reaction medium, the reaction temperature, the reaction time, and the ratio of the mole of sodium nitrite (n_NaNO2) to the mass of pectin (m_pectin) were 6, 60°C, 12 h, and 2.5/190 mol/g, respectively. Pectin and pectin sulfate were characterized by Fourier transform infrared (FTIR) spectroscopy and ¹³C‐NMR. The FTIR spectra showed the characteristic absorptions of sulfate ester bonds at 1264 and 830 cm^?1. Furthermore, the anticoagulant activity of pectin sulfates with different DSs, concentrations, and molecular weights were investigated with respect to the activated partial thromboplastin time (APTT), thrombin time (TT) and prothombin time. The clotting assay indicated that the pectin sulfate prolonged APTT and TT through inhibition of the activity of antithrombin. These results suggest that the introduction of sulfate groups into the pectin structure improved its anticoagulant activity. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

用气相色谱法测定丙烯醛水合加氢制备中的1,3-丙二醇

建立丙烯醛水合加氢制1,3-丙二醇的气相色谱定性定量分析方法。该分析方法能够准确地定量分析水合产物3-羟基丙醛和加氢产物1,3-丙二醇,相对误差为0.86%-1.89%,相对标准偏差为0.81%-3.21%,是一种快速、准确的分析方法。同时,通过分析数据能够计算反应的相关指标,为催化剂的研究评价和工艺条件的研究提供了依据。     

Hydration of tetracalcium aluminoferrite in presence of lime and sulfates

The first part of the paper describes conduction calorimetric and SEM studies of the initial first hour hydration of C₄AF and C₃A with water and saturated solutions of lime, gypsum and gypsum with lime. Lime accelerates while gypsum and gypsum with lime strongly retard the hydration of C₄AF. In case of C₃A, the effect is less pronounced. The second part deals with the hydration of C₄AF at later stages in presence of various additives and the same results as above are obtained. Anhydrite has very little influence while the presence of C₃A reduces the effect of gypsum and hemihydrate on hydration of C₄AF. A detailed investigation of the hydration process by means of X-RD, DTA, SEM and calorimetry has also been made.     

基于1,1-二溴-1-烯烃的对称1,4-二取代-1,3-二炔的合成

以1,1-二溴-1-烯烃为原料,DMSO为溶剂,通过Cs2CO3作用下的消除反应,首先生成炔基溴中间体。炔基溴中间体在Cu I/Et3N催化下再发生自偶联反应,"一锅法"合成了对称的标题化合物。相对于经典的Glaser反应,以易挥发且具有难闻气味的炔为原料合成对称性标题化合物,该合成方法以性质稳定、易于制备和便于操作的1,1-二溴-1-烯烃为原料,且反应收率较高,可作为传统Glaser反应的一种替代方法。