Sulfur chromatographic separation

Kremer L, Spicer LD. 1973. Gas chromatographic separation of hydrogen sulfide, carbonyl sulfide, and higher sulfur compounds with a single pass system. Anal Chem 45 1963-1964. 

Following extraction/cleanup, quinoxaline-2-carboxylic acid can be detected by electron capture, or mass spectrometric techniques, after gas chromatographic separation on capillary or conventional columns. A prerequisite of quin-oxaline-2-carboxylic acid analysis by gas chromatography is the derivatization of the molecule by means of esterification. Esterification has been accomplished with methanol (419, 420, 422), ethanol (421), or propanol (423) under sulfuric acid catalysis. Further purification of the alkyl ester derivative with solid-phase extraction on a silica gel column (422), thin-layer chromatography on silica gel plate (420), or liquid chromatography on Hypersil-ODS, 3 m, column (423), has been reported. 

With today s advanced analytical procedures, it is possible to describe the composition of these fuels in considerable detail. By combining several sequenced liquid chromatographic separations with gas chromatography-mass spectroscopy and by using specific gas chromatographic detectors for sulfur compounds, it has been possible to identify the majority of individual sulfur species in some fuels (12-19). A typical separation scheme is shown... 

Figure 14.3 Chromatographic separation of sulfur compounds in propene, obtained by using the system illustrated in Figure 14.2 1, hydrogen sulfide 2, carbonyl sulfide.

Figure 7. Ion chromatographic separation of ammonium ion (3) from sodium (1) and calcium (2) ions with a concentration ratio of sodium to ammonium of 60,000 1. Column Dionex CS15 eluent sulfuric acid and 18-crown-6. (from ref. 32)...

Hoshika, Y., Gas chromatographic separation of lower aliphatic primary amines as their sulfur-containing schiff bases using a glass capillary column, J. Chromatogr., 136, 253, 1977. 

Servigne, Y. and Duval, C., Paper chromatographic separation of mineral anions containing sulfur, Comput. Rend., 245, 1803, 1957 Chem. Abs., 52, 5207b, 1958. 

An earlier procedure reported from this laboratory for the isolation of sulfides was based on the selective oxidation of the sulfides to the sulfoxides with photoexcited singlet oxygen followed by silica gel chromatographic separation of the sulfoxides (9). Reduction of the isolated sulfoxides back to the sulfides and a subsequent chromatographic purification resulted in the isolation of the sulfides as a pale yellow oil. However, when the sulfur is in a five-membered ring, the photooxidation may lead to side reactions (22). Therefore, other oxidation methods had to be explored. 

Thomsberra, W. L. Isothermal gas chromatographic separation of carbon dioxide, carbon sulfide, hydrogen sulfide, carbon disulfide and sulfur dioxide. Anal. Chem. 

The references just cited provide only outline descriptions of the chromatographic separations. In this synthesis, detailed procedures are presented. The preparation requires 1 day for the sulfur chloride-ammonia reaction plus 2 to 7 days of intermittent attention (depending upon which imides are required) for the subsequent chromatographj and recrystallization. 

Steudel R., Holdt G., Gobel T., and Hazeu W. (1987) Chromatographic separation of higher polythionates (Sn)621 (n = 3...22) and their detection in cultures of Thiobacilus ferrooxidans molecular composition of bacterial sulfur secretions. Angew. Chemie. Int. Ed. Engl. 26, 151-153. 

Data on the separation of thietane by gas chromatography have been reported along with data on other sulfur compounds. Thin-layer chromatographic separation of thietane from 1,2-dithiolane and 1,2.3-trithiane works well on silica gel. Thietane forms a hydrate (dec 11.7°) with water. Its clathrate structure was investigated by use of the nmr line shapes of the deuterium oxide hydrate. ... 

By chromatography on silica gel 60 at a column temperature of -40 °C the 8x mixture has been separated into six fractions the mean molecular mass of the sulfur rings dissolved in these fractions ranged from 1100 (first fraction) to 733 (last fraction). In other words, 8 must contain rings with up to 35 atoms at least [88]. A more sophisticated chromatographic separation will be described in the following section. 

The production of HMF was even driven forward to a pilot plant scale including the work up and isolation of the pure product [34]. It consists essentially of the following steps (1) dehydration of fructose to HMF in aqueous solution (0.5 M) under sulfuric acid catalysis at 150°C (2) cooling and subsequent neutralization (CaOH or CaCOa) and filtration (3) chromatographic separation of the filtrate on calcium-loaded strong acidic cation exchanger resin and (4) cooling crystallization of the HMF fraction with overall HMF yields of 40-50%. 

Andersson, J. T., Retention properties of a palladium chloride/silica sorbent for the liquid chromatographic separation of polycyclic aromatic sulfur heterocycles. Anal. Chem., 59, 2207-2209, 1987. 

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