Impurities in Commercial Saccharin. I. Impurities Soluble in Organic Solvents

1976 ◽  
Vol 59 (5) ◽  
pp. 1051-1058 ◽  
Author(s):  
Bozidar Stavrić ◽  
Raymond Klassen ◽  
W Arnold

Abstract Thirteen saccharin samples used for carcinogenicity tests in animals in various laboratories were analyzed for their chemical purity. Although most of the impurities were water-soluble, some were mainly soluble in organic solvents. These impurities were extracted with chloroform-methanol from a water solution of sodium saccharin. Samples obtained as acid-saccharin were converted to the sodium form before extraction. The major impurity in commercial saccharin, o-toluenesulfonamide, was also soluble in this system. Impurities were separated by gas-liquid chromatography of the underivatized, concentrated extract. Eleven major, well separated peaks were collected from the gas chromatographic column and identified by mass spectroscopy. Some of the peaks were compared with known standards. Qualitative and quantitative differences in impurities were observed among different saccharin samples. The identified impurities (in order of appearance from the gas-liquid chromatographic column) were as follows: o-toluenesulfonamide; p-toluenesufonamide; 1,2-benzisothiazole 1,1-dioxide; 1,2-benzisothiazoline 1,1-dioxide; diphenylsulfone; o,o′-ditolylsulfone; o,m′-ditolylsulfone, o,p′-ditolylsulfone; m,p′-ditolylsulfone; p,p′-ditolylsulfone, and tetracosane.

1977 ◽  
Vol 23 (7) ◽  
pp. 1306-1309 ◽  
Author(s):  
R H Smith ◽  
J A MacDonald ◽  
D S Thompson ◽  
W E Flacke

Abstract We describe an isothermal gas-liquid chromatographic procedure developed for measuring thiamylal and thiopental in plasma. The unchanged drug is extracted into ethyl acetate from acidified plasma, together with an internal standard. The solvent is removed, the residue methylated, aliquots, diluted with benzene, are injected into a 183-cm gas-liquid chromatographic column containing 3% OV-17. Sensitivity of detection is in the nanogram to picogram range.


Author(s):  
Duy Hung Nguyen ◽  
Yu. V. Snigireva ◽  
A. V. Taneeva ◽  
V. F. Novikov

THE PURPUSE. The paper considers the influence of the nature of organic solvents on the process of separation of an antioxidant additive added to transformer oil at a concentration of up to 0.40% by weight, and organic solvents used as selective extractants. Based on the analysis of literature data, it is shown that mineral transformer oil is a complex hydrocarbon composition that undergoes oxidative degradation during operation, leading to aging of transformer oil and deterioration of technical conditions of operation of transformer electrical equipment. As a result of this process, peroxide compounds appear in transformer oil, which affect its color, oxidation stability, aging resistance, compatibility with structural parts of equipment, etc. Gas -liquid chromatography was used to determine the "Ionol" antioxidant additive and organic extractants in transformer oil. Experiments were performed on a chromatograph of Chromosomes GC -1000 with a flame ionization detector and a quartz capillary column 30 m long, 0.32 mm in diamet er, filled with a fixed liquid phase Valko Bond VB-WAX P/n with a film thickness of 0.5 microns. The sample was dosed into the gas-liquid chromatograph injector using an automatic liquid dispenser DAZH-23, designed for entering up to twenty-three samples of sorbates and controlled by a computer with the appropriate software.METHODS. Aliphatic alcohols from C1 to C5 were studied as extractants of the antioxidant additive, which are well separated from the ionol both under isothermal conditions and in the mode of linear programming of the column temperature from 40 to 220 °C. Under these conditions the chromatogram of the separation of antioxidant additives, and aliphatic alcohols, which are used to calculate their relative retained volumes, the asymmetry of chromatographic peaks and the column efficiency, which depends on the physico -chemical nature of the solutes to be analyzed and the conditions of the chromatographic experiment.RESULTS. The dependence of the relative volume of retention of aliphatic alcohols on their permittivity, which has a nonlinear form, is established. At the same time, with a decrease in the chain length of alkyl substituents in the aliphatic alcohol molecule, there is a tendency to increase their permittivity. The dependence of the relative retained volume of aliphatic alcohols on the selectivity coefficient of separation with Ionol is linear. In this case, the most optimal separation selectivity, approaching one, is characteristic of the Ionol – Butanol-1 pair. It is shown that the dependence of the logarithm of the retention time of aliphatic alcohols on their boiling points is linear both at a low temperature of the chromatographic column (40 °C) and at a higher temperature (more than 100 °C). CONCLUSION. At the same time, the angle of inclination of the corresponding lines changes in the boiling point of organic solvents, which is associated with a change in the sorption mechanism in a capillary chromatographic column filled with a polar stationary phase.


2022 ◽  
Vol 1212 (1) ◽  
pp. 012023
Author(s):  
A V Levina ◽  
A Ya Fedorov ◽  
M I Fedorova

Abstract The problem of e-waste processing and recovery of valuable metals from such waste for the second use is attracting more and more scientists’ attention. Liquid extraction as one of hydrometallurgy steps is a traditional method for the metal recovery. However, application of solvent extraction is not meet the green chemistry principles due to organic solvents. Aqueous two-phase systems based on water-soluble polymers are promising alternative for hazardous organic solvents. In this work the dependencies of Ce(III) and La(III) distribution coefficients from process time and the initial quaternary ammonium base concentration have been achieved. Also, based on the Ce(III) and La(III) extraction isotherms it has been shown that the metals initial concentrations are highly affects the distribution coefficients of studied metals. The possibility of aqueous two-phase system application as a solvent for quaternary ammonium salt for light REE (Ce(III) and La(III)) extraction from water solution has been shown.


1978 ◽  
Vol 24 (9) ◽  
pp. 1599-1602 ◽  
Author(s):  
R H Smith ◽  
M A Brewster ◽  
J A MacDonald ◽  
D S Thompson

Abstract We describe an isothermal gas-liquid chromatographic procedure developed for measuring procaine and chloroprocaine in plasma. The unchanged drug is extracted into toluene from alkalinized plasma, together with an internal standard. The solvent is removed, the residue redissolved in methanol, and aliquots are injected into a 91.5-cm gas-liquid chromatographic column containing 3% OV-210. Sensitivity of detection is in the nanogram range.


1979 ◽  
Vol 62 (6) ◽  
pp. 1309-1311
Author(s):  
Delbert D Oehler

Abstract A method is presented for the determination of permethrin (m-phenoxybenzyl cis,trans-(±)-3-(2,2-dichlorovinyl) - 2,2 - dimethylcyclopropanecarboxylate) in bovine tissues. Fat and muscle samples were cleaned up first by liquid-liquid partition on a bonded phase chromatographic column. Final cleanup of fat and muscle was performed on a short Florisil column. Liver, kidney, spleen, and heart tissues only required cleanup on a Florisil column before quantitation of permethrin by electron capture gas-liquid chromatography.


1980 ◽  
Vol 26 (10) ◽  
pp. 1480-1483 ◽  
Author(s):  
F Chow ◽  
A Karmen

Abstract Compounds with primary amino groups react with o-phthalaldehyde in solution to yield highly fluorescent products. This reaction is now in wide use for detecting amino acids and amines in liquid-chromatography effluents. We report here a method for using o-phthalaldehyde to detect primary amines in the effluent of a gas-liquid-chromatographic column. The effluent gas, nominally 20 mL/min, is delivered to a scrubber consisting of a small-bore, simulated capillary chromatographic column that is simultaneously supplied with 1 mL/min of the reagent solution. The liquid effluent of the scrubber, separated from the gas, is drawn through the flow cell of a fluorometer. Short-chain amines and ammonia were quantitatively scrubbed. The response of the fluorometer was directly proportional to the number of nanomoles injected into the column. Less than a nanomole of amine was detectable. Comparison of results with those from a hydrogen flame-ionization detector showed minimal additional peak broadening or compromise of resolution. These results demonstrate the feasibility of using highly specific, as well as sensitive, liquid-chromatographic detection methods for gas-liquid chromatography.


1993 ◽  
Vol 58 (10) ◽  
pp. 2321-2336 ◽  
Author(s):  
Zhong-wei Gu ◽  
John D. Spikes ◽  
Pavla Kopečková ◽  
Jindřich Kopeček

In cancer photodynamic therapy (PDT), improved efficiency of photosensitizer delivery to tumors may be obtained by binding them to targetable water soluble polymeric carriers. However, attachment of photosensitizers to Macromolecular carriers may alter their spectral and photosensitizing properties. In this study, a new monosubstituted phthalocyanine derivative, N-glycyl zinc(II) 4,9,16,23-tetraaminophthalocyanine (G-TAPC-Zn) was synthesized by the reaction of zinc(II) 4,9,16,23-tetraaminophthalocyanine (TAPC-Zn) with N-tert-butoxycarbonyl-glycine N'-hydroxybenzotriazole ester followed by deprotection of the tert-butoxycarbonyl (BOC) group. G-TAPC-Zn contains an aliphatic amino group suitable for attachment to water soluble polymeric carriers. By aminolysis of a polymeric precursor, an N-(2-hydroxypropyl)methacrylamide (HPMA) copolymer containing oligopeptide (GFLG) side-chains terminated in p-nitrophenyl ester groups, with G-TAPC-Zn a polymeric derivative of the latter (P-GFLGG-TAPC-Zn) was synthesized. Spectral data indicated that in aqueous solutions P-GFLGG-TAPC-Zn formed aggregates. The degree of aggregation decreased with increasing concentration of detergents or organic solvents in buffer solutions. Consequently, the release of the drug from carrier catalyzed by thiol proteinases, papain or cathepsin B, took place only in the presence of detergents or organic solvents, i.e., under conditions with a lower probability of aggregate formation. Binding of G-TAPC-Zn to HPMA copolymers decreased the quantum yield of singlet oxygen generation from 0.24 to 0.063 and significantly increased its resistance to photobleaching.


Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1316
Author(s):  
Vanessa Miglio ◽  
Chiara Zaccone ◽  
Chiara Vittoni ◽  
Ilaria Braschi ◽  
Enrico Buscaroli ◽  
...  

This study focused on the application of mesoporous silica monoliths for the removal of organic pollutants. The physico-chemical textural and surface properties of the monoliths were investigated. The homogeneity of the textural properties along the entire length of the monoliths was assessed, as well as the reproducibility of the synthesis method. The adsorption properties of the monoliths for gaseous toluene, as a model of Volatile Organic Compounds (VOCs), were evaluated and compared to those of a reference meso-structured silica powder (MCM-41) of commercial origin. Silica monoliths adsorbed comparable amounts of toluene with respect to MCM-41, with better performances at low pressure. Finally, considering their potential application in water phase, the adsorption properties of monoliths toward Rhodamine B, selected as a model molecule of water soluble pollutants, were studied together with their stability in water. After 24 h of contact, the silica monoliths were able to adsorb up to the 70% of 1.5 × 10−2 mM Rhodamine B in water solution.


2016 ◽  
Vol 871 ◽  
pp. 96-103 ◽  
Author(s):  
Vladimir Erofeev ◽  
Aleksandr Bobryshev ◽  
Aleksandr Lakhno ◽  
Lenar Shafigullin ◽  
Ilnaz Khalilov ◽  
...  

Presents the results of studies of contemporary materials in the field of rheological state. The topological mortar structure has been provided by theoretical evaluation of the rheological state of the cross-linked solutions and the experimental viscosity data of the sand cement mortar which has been modified by water-soluble additive – polyoxyethylene. The general model has been made for the structure of non-Newtonian liquideous systems including dilatant, pseudoplastic bodies with two main rheological active components in their structure – rigid and viscous phases. It is shown that in pseudoplastic systems, as the shear stress increases, the viscous phase grows because of the reduction of rigid phase content. In dilatant systems the converse situation has been observed. Furthermore, these phases are not clearly distinguishable, but to the contrary they are spatially interconnected in a complex way. The structure modeling has been made for non-Newtonian bodies using the Shklovskii-de Gennes model. The studies have found that the construction composite sand cement system is defined as the pseudoplastic body where cement and sand act as the rigid phase, water solution of polyoxyethylene – as the viscous phase. These findings can be used to prove the influence of polymer powder on the workability of dry mortar.


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