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By T. R. Crompton

Since its creation into the armoury of the analytical chemist nearly twenty years in the past the means of gasoline chroma­ tography has discovered very wide functions within the research of such a lot sorts of natural compounds. one of many few last barriers of the strategy whilst utilized to such compounds, particularly the research of very hugely boiling and or thermally volatile elements, has been conquer sometimes by way of the creation of thoughts akin to silation for the conversion of pattern elements to reduce boiling or extra sturdy elements that are fuel chromatographed at kind of low temperatures. All of this has been widely handled in lots of books released in the course of contemporary years facing the speculation and perform of using fuel chromatography to the research and preparative separation of natural compounds. In parallel with those advancements there has happened, particu­ larly over the last decade, a turning out to be curiosity within the software of gasoline chromatography to the research of organometallic compounds. certainly, for lots of kinds of organometallic compounds, gasoline chromatography is the analytical approach to selection fairly, as so frequently occurs, whilst the pattern is a combination. To the author's wisdom no entire evaluate exists of the broadcast paintings during this very attention-grabbing new box; a scenario it's was hoping the current quantity will rectify.

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Different derivatives were prepared from portions of the purified extracts by treatment with dithizone, hydrobromic acid, potassium iodide or potassium cyanide. The dithizonates formed had the same Rf-va1ue as ethylmercury dithizonate using thin-layer chromatography on aluminium oxide (Figure 10). Furthermore, when the dithizonates from the fish samples were eluted from the spots on developed thin-layer chromatographic plates and gas chromatographed peaks with the same retention time as for methylmercury chloride were obtained.

This indicated a synthesis of methylmercury ions from mercuric ions by the liver under the conditions used. Thus, this combined mercuric ion-cysteine acetate procedure for analysis of methylmercury could not be applied to liver. Some results obtained without addition of methylmercury compounds are seen in Table 15. For egg-yolk with low content of methylmercury the cysteine acetate procedure gave less than 90% recovery48, (Method B described earlier). with the combined method using cysteine and mercuric ions the recovery of methylmercury salt decreased almost to zero.

Method 3. Finally, the purified extracts of methylmercury used in the gas chromatographic analysed of methylmercury developed by Westoo 48 (cysteine procedure) were ananlysed without further purification or concentration. All the samples were submitted to a combined gas chromatographmass spectrometer (LKB 9000), and both the direct and gas chromatograph inlets were used for these analyses. The samples were compared with equivalent amounts of methylmercury standards. 5mm Carbowax 20M Chromosorb W, 80 - 100 mesh Helium 30ml/min l40 0 C 200 0 C 200 0 C Mass spectrometer: Accelerating voltage Electron energy Electron current 3500v 70eV 60~a For extract concentrations of lng Hg/~l or lower, 10~1 of the solution were injected into the column of the combination instrument.

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