钒氮合金化学分析方法.docVIP

飢氮合金化学分析方法 Disti11ation separation and titration to determine the amount of nitrogen scope This standard stimulates the distillation separation medium and the method of titration determination of nitrogen content in the feed, reagents and materials, apparatus and equipment, analysis steps, the analysis results of calculation. This standard is applicable to the determination of nitrogen content in vanadium n alloy, measuring range (quality score): 1% to 30%. methods feed Sample with perchloric acid decomposition, the nitrogen into the corresponding amine salt, in under the action of excessive alkali, water vapor distillation separation of ammonia, the steam absorption boric acid solution for a fluid, with methylene blue as an indicator, methyl red - time with amino sulfonic acid standard solution titration. Three reagents All reagents should be reagents with low nitrogen content, all water with no ammonia? perchloric acid (p 1. 67 g/mL) Sodium hydroxide solution (50 g/L) 3.2: according to take 250 g sodium hydroxide in 500 ml plastic beaker, add 300 ml water, zinc addend grain, heat to boil for 10 min, residual zinc granule, refuse to remove cooling, diluted to 500 ml, blending. Reserve in plastic bottles? 3.3 boric acid absorption fluid (lg/L) 3. 4 amino-sulfonate (NH2S03H)二 0.1000 molar Weigh and 9. 7090 g in advance in sulfuric acid drying in vacuum drying 48 h the benchmark of amino sulfonic acid, put in 250 ml beaker, add water to dissolve, out into a 1000 ml volumetric flask and diluted with water to the scale, blending? Methyl red methyl blue indicator: 0. 125 g methyl red and 0. 083 g times methyl blue, soluble in lOOmL of ethanol, stored in brown flask? Four instruments Steam distillation apparatus (see figure 1) Any distillation apparatus that satisfies the following conditions shall be adopted: A. must be steam distilled: Rate of distillation: 70 、 lOOmL of liquid in 10 ~ 20min. C. Nitrogen recovery: 10 1500 u g nitrogen, 80 ml of liquid, and the recovery