Gas chromatographic analysis of nonionic surfactants by acid cleavage of ether linkages

The gas chromatographic analysis of various kinds of nonionic surfactants has been carried out after chemical decomposition using the mixed anhydride of acetic and p-toluene sulfonic acids which acts as a reagent for cleavage of ether linkages. The gas chromatographic peaks of the reaction products show the alkyl distributions of the hydrophobic groups of ethylene oxide adducts. The alkyl compositions closely agree with those of the starting materials. In this way, the hydrophobic groups of polyoxyethylene alkyl ether, polyoxyethylene alkyl phenol ether, polyoxyethylene alkyl amine, and polyoxyethylene alkyl thioether have been analyzed. At the same time, the hydrophilic group, namely polyoxyethylene group, can be identified in the form of ethylene glycol diacetate.     

表面活性剂复配体系修复芘污染土壤实验

以芘污染土壤为对象,利用阴离子表面活性剂鼠李糖脂和非离子表面活性剂皂素进行复配实验,得出最佳复配比并对污染土壤进行修复处理;其次,研究表面活性剂浓度、pH及CaCl₂、MgCl₂、KCl三种离子浓度、洗脱液的回收次数等单因素对洗脱效果的影响;然后利用响应曲面分析,确定影响洗脱效果的主效应因素及其交互作用强度;最后用Box-Behnken模型优化复配体系处理芘污染土壤的实验条件。结果表明：①当复配比为0.2时,鼠李糖脂-皂素混合溶液的表面张力最低,对芘的协同增溶效果最好;②复配体系处理芘污染土壤的单因素实验中,复配药剂浓度、pH、Mg²⁺浓度分别达到1800mg/L、8、0.1mmol/L时,洗脱效率最高;③环境因素对芘去除效果的影响从大到小依次为pH>表面活性剂浓度>Mg²⁺浓度,表面活性剂浓度与pH对芘的洗脱产生较大的交互影响作用,而pH与盐浓度的交互作用最微弱;④Box-Behnken模型优化后得出最佳组合是混合表面活性剂浓度为1900mg/L、pH为5、Mg²⁺浓度为0.2mmol/L,得到的洗脱效率为89.25%。     

Method for determination of combined maleic anhydride in rosin-maleic anhydride adducts by chromatographic techniques

A new analytical method for the determination of combined maleic anhydride in rosin maleic anhydride adducts has been developed. The method is based on the use of chromatographic techniques for separating the rosin acids and the rosin maleic anhydride adduct using silicic acidcelite as the adsorbent and benzene and acetone as solvents. An acid number is determined on the adduct which is used to calculate the combined maleic anhydride in the sample. Free maleic anhydride does not interfere in the analysis. Data are presented showing good agreement with the results obtained on known blends by infrared spectroscopy and chromatography.     

Gas chromatographic analysis for alpha-olefin sulfonate

The separation and determination of alkene sulfonate and hydroxyalkane sulfonate, and the carbon chain distribution of the lipophilic groups of long chain alpha-olefin sulfonates (C₁₄ to C₁₈) were studied by means of gas chromatography. Samples were hydrogenated initially, and converted to sulfonyl chlorides for gas chromatographic analysis. Using a glass column, 4 mm i.d. and 2.5 m long, packed with Silicon SE-30, 3% on 60 to 80 mesh Chromosorb WAW treated with hexamethyldisilazane, a 0.3 to 0.6 μl sample, as 10% carbon tetrachloride solution, was injected directly on the column, and alkane and monochloroalkane sulfonyl chloride were determined as alkyl chloride and alkyl dichloride, respectively. Minimization of further decomposition, improvement of peak separation and reproducibility were accomplished by this procedure. The method was applied to alpha-olefin sulfonates produced commercially from C₁₄ to C₁₈ alpha-olefins.     

Dimer acids: Gas chromatographic analysis

A gas chromatographic method is described for analyzing commercial polymerized fatty acids. The method determines unpolymerized acid, dimerized acid, and trimerized acid. Involved is an esterification to the methyl esters, followed by programed temperature gas liquid chromatography. Several years experience with this analysis has demonstrated its utility as a tool for quality control and research.     

Enhanced triolein removal using microemulsions formulated with mixed surfactants

In previous work, a microemulsion-based formulation approach yielded excellent laundry detergency with hydrophobic oily soils hexadecane and motor oil. In this work, the same approach is used in detergency of triolein, which is a model triglyceride, some of the most difficult oils to be removed from fabric. The linker concept was applied in formulation of the microemulsion system. Three different surfactants were used: (i) dihexyl sulfosuccinate, an ionic surfactant with a moderate hydrophile-lipophile balance (HLB); (ii) secondary alcohol ethoxylate, a lipophilic nonionic surfactant with a very low HLB; and (iii) alkyl diphenyl oxide disulfonate (ADPODS), a hydrophilic anionic surfactant with a very high HLB. The phase behavior and interfacial tension (IFT) of the surfactant systems were determined with different concentrations of ADPODS. The results indicate that as the HLB of the system increases, a higher salinity is required to shift the phase transition from Winsor Type I to Type III to Type II. The three formulations at different salinities were used in detergency experiments to remove triolein from polyester/cotton sample fabric. The results showed that there were two peaks of maximum detergency in the range of salinity from 0.1% to 10% NaCl. The higher the hydrophilicity of the system, the higher the salinity required for maximum detergency. The results of the dynamic IFT and the detergency performance from two rinsing methods lead to the hypothesis that one of these maxima in detergency results from a spreading or wetting effect. The other maximum in detergency is believed to be related to ultralow IFT associated with oil/water middle-phase microemulsion formation. Triolein removal exceeding 80% was attained, validating the microemulsion approach to detergency.     

2-氯乙基氨基甲酸乙酯气相色谱分析

采用气相色谱法，柱填充物为3％OV-101涂渍在Chromosorb W AW DMCS080～250μm）上，柱温：190℃，气化室：230℃，检测室：230℃；内标物为联苯，用内标法对2-氯乙基氨基甲酸乙酯有效成分进行分离和检验。方法标准偏差≤0．31，变异系数〈0．32，平均回收率为99．86％。     

1，6-己二醇二丙烯酸酯（HDDA）的气相色谱分析

气相色谱法分析HDDA的含量。以SE-54毛细管柱为固定相，氢火焰离子检测器、程序升温。该方法操作简便、快速、灵敏、精密度高、准确度好，适用于HDDA的分析。     

“Acid” pyrolysis-capillary chromatographic analysis of anionic and nonionic surfactants

A tandem “acid” pyrolysis-capillary chromatographic method for analyzing surfactants has been developed, and its application to the more common anionic and nonionic surfactant types investigated. In this method a surfactant is mixed with an acid, such as P₂O₅ or H₃PO₄, and dropped into a pyrolyzer attached to a capillary gas chromatograph. The resulting volatile pyrolyzate is carried into the chromatograph for analysis. According to the chromatograms, the point of cleavage during “acid” pyrolysis is quite selective, usually at a C-S or C-O bond. For example, LAS and ABS give peaks corresponding to the alkylbenzene precursors; primary linear alkyl sulfates and sulfonates, peaks corresponding to olefins with the same number of carbon atoms as the alkyl group; and alcohol and alkylphenol ethoxylates and ethoxylate sulfates, peaks corresponding to olefins from the alkyl group and to acetaldehyde and a higher aldehyde from the polyethoxy group. Alkylphenol derivatives are probably cleaved to form an alkylphenoxy intermediate, which then dealkylates to give the olefins. This method is quantitative for carbon number or carbon number and isomer distribution of hydrophobes in linear surfactants, semiquantitative for ethoxy content and for hydrophobes in branched chain surfactants, and qualitative for hydrotropes and certain foam additives. Surfactants, as well as mixtures of certain surfactant types, in built detergent formulations can be analyzed without isolation. Winner, Bond Award Medal, Philadelphia, October 1966.     

3-溴-4-氟苯甲醛的气相色谱分析方法

采用气相色谱法,氢火焰离子化检测器,选用3%OV-17填充柱,正十三烷为内标,气化室和检测器温度为180℃,柱温120℃,对3溴4氟苯甲醛进行定量测定。该方法简单、快速、准确、适用,标准偏差0.26%,变异系数0.27%,平均回收率100.1%。     

气相色谱法分析气体中组分的加速

通过对气相色谱法分析气体样品N2、CO、CH4、CO2的实验方法中进样阀动作时间做相应的调整,第1次动作,第1个样品进样;第2次动作,第2个样品开始置换;第3次动作,第2个样品进样;第4次动作,阀复位到初始状态。在满足各色谱峰能够完全分离且分离度大于1.5的条件下,在对多个样品进行分析时,可以节省分析时间43%,RSD<0.010%。     

Preparation of epoxy acrylate emulsion using mixed surfactants and its polymerization

Summary A series of epoxy acrylate emulsions were prepared with several surfactants ranging from HLB 12 to 14 at 40°C. For epoxy acrylate emulsion, additives and conditions were established among factors: HLB value of emulsion, agitation speed, water dropping speed, and dropping amount of the deionized water. For emulsion polymereization with water soluble initiator KPS, emulsion was broken during polymerization, because interfacial complex formed by association of surfactant with co-surfactants stabilizing emulsion was weakened by interpenetration of radicals formed at aqueous. Accordingly, the polymerization of epoxy acrylate emulsion was carried out by using oil soluble initiator, AIBN, and the conversion changes with initiator concentration and HLB values were investigated.     

Removal of Ni(II) ions from wastewater by micellar enhanced ultrafiltration using mixed surfactants

Ni(II) ions were removed from aqueous waste using micellar enhanced ultrafiltration (MEUF) with a mixture of surfactants. The surfactant mixture was the nonionic surfactant Tween 80 (TW80) mixed with the anionic surfactant sodium dodecyl sulfate (SDS) in different molar ratios ranging from 0.1–1.5. The operational variables of the MEUF process such as pH, applied pressure, surfactant to metal ion ratio and nonionic to ionic surfactant molar ratio (α) were evaluated. Rejection of Ni and TW80 was 99% and 98% respectively whereas that for SDS was 65%. The flux and all resistances (fouling resistance, resistance due to concentration polarization) were measured and calculated for entire range of α respectively. A calculated flux was found to be declined with time, which was mainly attributed to concentration polarization rather than resistance from membrane fouling.     

Gas chromatographic analysis of fragrances in palm-based white soaps

Four commercial soap fragrances 1,2,3, and 4 were incorporated in palm-based white soaps and made into bars. The soap bars were stored at 25°C and 40°C for three months. The headspace gas-chromatographic volatiles, fragrance odor intensity and whiteness analyses of the soap samples were carried out at 10-day intervals. By means of gas chromatography and mass spectrometry, some of the headspace gas-chromatographic peaks were identified. These peaks were useful in monitoring the fragrance components. For example, fragrance 4 contains the components limonene and citronellal which are known to possess a citrus odor component. Fragrance odor intensity scores showed that the intensity of the fragrances in the soap base was the same for all. Results also showed that most of the fragrances had the same effect on the whiteness of palm-based white soaps, except for fragrance 2 which gave a pink color to the white soaps. Equations were established between the fragrance odor intensity and area under the gas-chromatographic peaks. The equation can give useful information on the fragrance odor intensity by calculating the area of the chromatographic peaks; the fragrance odor intensity is a reflection of the fragrance retention in palm-based soaps.     

Gas chromatographic analysis of cyclopropenoid acids in cottonseed oils

A gas chromatographic method of analysis for cyclopropenoid acids in cottonseed oil, as the methyl esters, is described. With a glass column packed with a methyl silicone substrate on an inert support, methyl sterculate and methyl malvalate can be chromatographed without decomposition. Although methyl malvalate was not well resolved from methyl linoleate, it could be quantitated accurately at concentrations as low as 0.03% by a peak-height method. Quantitation can be done manually with an internal standard, or with a data system without an internal standard. The method does not require calibration with a cyclopropenoid acid standard, i.e., it is a primary method. Results compare favorably with those obtained by HBr titration. Less than 1 mg of oil is required for an analysis. Retired.     

混合表面活性剂体系合成锆掺杂介孔分子筛

在水热体系中研究了以阳离子表面活性剂为主,阴离子表面活性剂、非离子表面活性剂、中性伯胺等为辅的混合表面活性剂对合成锆掺杂介孔分子筛的影响,考察了水/SiO2摩尔比、晶化温度、晶化时间及混合表面活性剂/SiO2摩尔比对所制分子筛结构的影响,对优化条件下合成的样品进行了表征. 结果表明,锆掺杂介孔分子筛的最佳合成体系为阴阳离子表面活性剂混合体系,最佳合成配方为水/SiO2摩尔比58,混合表面活性剂/SiO2摩尔比0.15, 100℃下晶化48 h. 最佳条件下合成的样品在小角区域有一个明显的衍射峰,表明其具有一定的长程有序性,晶面间距d=9.71 nm,平均孔径为5.55 nm,壁厚4.16 nm,具有三维蠕虫状孔道结构,吸附亚甲基蓝、罗丹明B与甲基橙的混合溶液时,对亚甲基蓝的吸附选择性较好,吸附率达90.24%.     

2-氨基-4,6-二甲基嘧啶的气相色谱分析

用气相色谱法对2-氨基-4，6-二甲基嘧啶进行了分析方法的研究。线性范围0．26-0．78mg／mL，相关系数r＝0．99662，加标回收率101．8％-106．3％，相对标准偏差0．20，变异系数0．21％。该方法简单、快速、结果准确，可作为质量控制的检测方法。     

Esterification of styrene–maleic anhydride copolymer by mixed alcohols

A copolymer (MW = 1800) of styrene (St) and maleic anhydride (MAn) was esterified with an excess amount of an alcohol mixture, and then the relation between the esterification rates of the individual alcohols and the contents of the esters in the esterific copolymer was examined. At first, the rate constant of an individual esterification was obtained for four different alcohols (n-butanol, i-amylalcohol, and benzylalcohol) in a noncatalyst system. Then, the mixed esterification of n-butanol and i-amylalcohol was carried out; from the analysis of the ester contents, the following equation was obtained: From this result, it was concluded that, in esterification with alcohols involving n species, the content of the individual ester can be expressed by the following equation: where [P] = concentration of esters in the copolymer, [B]₀ = initial concentration of alcohols, and k = rate constant of esterification (i,j = 1,2…,n).