Thin-layer chromatograms

As for paper chromatograms, thin layer plates may be placed in a tank containing scintillator and covered with x-ray film. This procedure is unsuitable for fragile adsorbents or for substances which diffuse or dissolve in the scintillator solvent. 

Total ion current chromatogram Thin layer chromatography 1,3,6-Trioxocane... 

Purified by chromatography on a column of deactivated alumina or magnesium oxide, or on a thin layer of silica gel G (Merck), using dichloromcthane/dicthyl ether (9 1) to develop the chromatogram. Stored in the dark and in an inert atmosphere at -20 . 

Referring again to the retention of a solute on a thin layer plate depicted in figure 2 and comparing this with a normal GC or LC chromatogram, then the distance (y - x)... 

It is only since this method has come into use that the precise quantitative analysis of thin-layer chromatograms has become possible. For the increased... 

Color reproduction of the chromatograms can be achieved by color photography — the best, but also the most expensive method of documenting thin-layer chromatograms. It can be used not only to produce true-color reproductions of colored zones but also — with the aid of a Reprostar (Fig. 64) or a UVIS analysis lamp (Fig. 6) — of fluorescent or fluorescence-quenched zones. When photograph-... 

The blue-violet stain which forms on thin-layer chromatograms when amino acids are stained with ninhydrin is only stable for a short time. It rapidly begins to fade even on cellulose layers. The stability can be appreciably enhanced by complex formation with metal ions [3]. 

The first part of the book consists of a detailed treatment of the fundamentals of thin-layer chromatography, and of measurement techniques and apparatus for the qualitative and quantitative evaluation of thin-layer chromatograms. In situ prechromatographic derivatization techniques used to improve the selectivity of the separation, to increase the sensitivity of detection, and to enhance the precision of the subsequent quantitative analysis are summarized in numerous tables. 

Funk et al. have used a low-pressure mercury lamp without filter to liberate inorganic tin ions from thin-layer chromatographically separated organotin compounds these were then reacted with 3-hydroxyflavone to yield blue fluorescent chromatogram zones on a yellow fluorescent background [22]. Quantitative analysis was also possible here (XoK = 405 nm, Xji = 436 nm, monochromatic filter). After treatment of the chromatogram with Triton X-100 (fluorescence amplification by a factor of 5) the detection limits for various organotin compoimds were between 200 and 500 pg (calculated as tin). 

Reactions can be exploited more speciHcally if it is known that particular functional groups are present [cf. Chapter 2]. They still do not allow direct identification, but they increase the specificity of the evidence. The chromatographic separation carried out before detection also contributes to this. This reduces the number of potential components. However, this does not exclude the possibility that there might be several substances in the particular part of the chromatogram involved. This not only applies to thin-layer chromatography but also applies with equal force to other microanalytical separation methods (GC, HPLC). 

Note When combined with thin-layer chromatographic separation the reagent provides a specific detection method for nitrate and nitrite. The color development is often completed within a few minutes on silica gel plates. In the absence of ammonia vapor traces of oxides of nitrogen in the laboratory atmosphere can slowly cause the background to become reddish-brown. The simultaneous presence of the following ions in the chromatogram zones interferes with the detection of nitrate/nitrite I , 10J, IO4, MoO and H2PO2. 

Fig. 1 Thin-layer chromatogram of triazines (amount applied 4 gg each substance per chromatogram zonelflVacks 1 and 5 = mixture. Track 2 = cyanazin, Track 3 = terbutylazin. Track 4 = anilazin.

Analysis calculated for C1SH36N2O4S C, 57.41 H, 9.63 N, 7.43 S, 8.51. Found C, 57.60 H, 9.66 N, 7.37 S, 8.25. Thin-layer chromatograms (Note 10) run by the submitters showed a single spot for the product in each of three following solvent systems (solvents, volume ratio of solvents in the same order) chloroform-methanol-acetic acid, 85 10 5, Rf 0.60 1-butanol-acetic acid-water, 4 1 1, Rf 0.58 l-butanol acetic acid-pyridine-water, 15 3 10 12, Rf 0.71. 

The literature reports [a]n +23.2° (c = l, aqueous 5N hydrochloric acid). The product was analyzed by the submitters. Analysis caleulated for C5H11NO2S C, 40.25 H, 7.43 N, 9.39 S, 21.49. Found C, 40.14 H, 7.42 N, 9.50 S, 21.52. The product was homogeneous according to thin-layer chromatograms on precoated silica gel G plates purchased from Analtech, Inc., Newark, Delaware, and developed with the following two solvent systems (solvents, volume ratios of solvents in the same order) 1-butanol-acetic acid-ethyl acetate-water, 1 1 1 1, Rf 0.49 1-butanol-acetic acid-pyridine-water, 15 3 10 12, R/0.51. 

Thin-layer chromatograms were run on plates coated with silica gel using 1 10 (v/v) ether-hexane as developing solvent. 

Recendy the Ar /He—Ne lasers have been employed for the analysis of thin-layer chromatograms [259 — 261]. However, instruments of this type have not yet come into general use. 

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