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.     

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.     

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。     

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％。     

“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%。     

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.     

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.     

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。     

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.     

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).     

Gas chromatographic analysis of the dimethylhydrazones of long chain aldehydes

Long chain saturated and unsaturated aldehydes, prepared by the partial reduction of the corresponding fatty acid phenyl esters with lithium tri-t-butoxyhydroaluminate, were converted quantitatively to their dimethylhydrazones. Dimethyl acetals and 1,3-dioxolanes were prepared from the dimethylhydrazones. The dimethylhydrazones were then separated from the corresponding aldehydes by gas liquid chromatography on a semipolar column. Fatty acids were readily separated quantitatively from fatty aldehydes by formation of dimethylhydrazones of the aldehydes followed by an alkaline extraction of the reaction mixture prior to gas chromatography. A method for analysis of fatty acids and aldehydes from plasmalogens is described. Presented at the AOCS Meeting, Chicago, October 1967. Michigan Agricultural Experiment Station Journal Article No. 5104.     

苯酐氯化制单氯代苯酐

介绍了以苯酐、C l2为原料,无水FeC l3做催化剂,制备单氯代苯酐的方法,从苯酐的转化率、单氯代苯酐选择性两方面展开了苯酐氯化制备单氯代的研究,指出最佳的制备条件为:催化剂用量1.5%,C l2与苯酐摩尔比0.8∶1,反应时间11h。     

40%三唑磷水乳剂的气相色谱分析方法

采用气相色谱法分析40％三唑磷水乳剂,固定相为1．5％SE-30,内标物为邻苯二甲酸二环己酯,三唑磷色谱峰与内标物色谱峰的分离度为3．0。方法的相关系数为0．9996,标准偏差为0．0689,变异系数为0．17％,平均回收率为99．8％。     

敌稗·(口恶)草酮复配制剂的气相色谱分析

介绍了在HP-1(30m×0.53mm×1.50μm)大口径毛细柱上以邻苯二甲酸二戊酯做内标,进样口和检测器温度均为250℃,在柱温220℃下进行分离,用FID检测器对敌稗·草酮复合制剂进行气相色谱定量分析的方法。两种有效成分敌稗、草酮在同一条件下测定,操作简便,方法的线性相关系数均为0.9999,精密度和准确度较好。