Quantitative analysis of nitro compounds
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I have been working on nitro compounds recently, and some impurities in the liquid chromatography results do not show up as peaks. Therefore, I want to use chemical methods to determine the content of these nitro compounds. I’ve looked up some information, and the quantitative analysis methods for nitro compounds mentioned there are: 1. reduction titration with titanium trichloride, 2. reduction titration with stannous chloride, 3. reduction with zinc powder followed by diazotization titration. The first two methods involve experimental procedures, but due to limitations in experimental conditions and my product, they are not very suitable. Therefore, I would like to use the third method. However, no information is available regarding the process of reducing nitrocompounds using zinc powder, so I would like to ask the experts here if they could tell me the specific steps for carrying out this reduction process. Thank you.
What type of nitrocompound is it? For *** types, if the concentration is high: an appropriate amount of the substance to be tested is added to an excess of zinc powder along with 20 milliliters of 1:1 hydrochloric acid. The mixture is heated under reflux with a condenser to ensure complete reaction; after cooling to room temperature, it is titrated using sodium nitrite, with starch-iodide paper as an indicator. For low concentrations, the naphthylethylenediamine hydrochloride colorimetric method is used.
Thank you. Mine is a high-concentration *** compound, with over 80% being nitro compounds. Could you be more specific and detailed?