By L. Mázor
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Additional resources for Analytical Chemistry of Organic Halogen Compounds: International Series in Analytical Chemistry
In this method the organic substance is decomposed with concentrated nitric acid in a thick-walled b o m b at 3 0 O - 3 5 0 ° C . In the 1 5 to 2 0 - m l microbomb, about 1 0 mg of the sample is treated with 0 . 5 to 1 ml of concentrated nitric acid. Silver nitrate is also added t o react with the halide ions formed. The description of the practical realization of the procedure is omitted, because it is rather timeconsuming and it is applied mostly in conjunction with quantitative micro determination of halogens, rather than for qualitative detection purposes.
The detection of halogens in gaseous or very volatile compounds requires special decomposition procedures. , C u O or C03O4 at 400-600°C). Then the halogen or hydrogen halide produced is absorbed in water or alkaline solutions or other suitable absorbent. Chlorine, bromine and iodine are usually retained on metallic silver layers; magnesium oxide is used for fluorine; they are later dissolved from the surface and detected. As the strength of the carbon-halogen bond can vary widely in organic halogen compounds, for unknown substances the most powerful decomposition reagent should be used to avoid partial or unsuccessful decomposition.
The apparatus shown in Fig. , 12 m m long) made by rolling a thin copper sheet into a tube. This is soldered t o the small-diameter end of a glass tube attached to a town gas supply. The gas gives a microflame at the end of the copper tube and the part within 1-2 m m of the end of the tube glows red-hot. The solid substance to be tested is placed in the glass tube at point 1 (a small platinum boat can be used for this purpose) and evaporated rapidly by heating with a microburner (the gas flow is adjusted so as to obtain a flame 3-4 m m long).