钒氮合金化学分析方法（Methods for chemical analysis of vanadium nitrogen alloys）.docVIP

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钒氮合金化学分析方法（Methods for chemical analysis of vanadium nitrogen alloys）.doc

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钒氮合金化学分析方法（Methods for chemical analysis of vanadium nitrogen alloys）

钒氮合金化学分析方法（Methods for chemical analysis of vanadium nitrogen alloys） Distillation separation - Determination of nitrogen content by neutralization titration 1 range This standard specifies a method for the determination of nitrogen content by a neutralization titration in distillation. The feed, reagents and materials, apparatus and equipment, analytical procedures, and calculation of analytical results. This standard applies to the determination of nitrogen in vanadium nitrogen alloy, measuring range (mass fraction):1%-30%. 2 method summary With perchloric acid sample, the nitrogen into the corresponding amine salt in excess alkali under the effect of steam distillation of ammonia, boric acid solution absorption distillation liquid, using methyl red methylene blue as the indicator, titration with sulfamic acid standard solution. 3 reagent All reagents should use reagents with low nitrogen content, all water is ammonia free water. 3.1 perchloric acid (P, 1.67g / mL) 3.2 sodium hydroxide solution (50g / L): 250g NaOH in 500mL plastic beaker, add 300mL of water, boil the addend zinc particle particle, 10min, discarding the residual zinc particles, remove the cooling, dilute with water to 500mL and mix. Keep it in a plastic bottle. 3.3 boric acid absorption solution (1g/L) 3.4 amino sulfonic acid standard solution [C (NH2S03H) =0.1000mol / L] Take 9.7090g as the standard amino acid for drying 48h in a vacuum drying of sulfuric acid. Place it in a 250mL beaker, dissolve in water, and move into a 1000mL volumetric flask. Dilute with water until the scales are mixed. 3.5 methyl red methylene blue indicator: 0.125g and 0.083g of methyl red methylene blue 100mL, soluble in ethanol, stored in a brown bottle. 4 instrument Steam distillation apparatus (see Figure 1) Any instrument that satisfies the following conditions may be used: A. must be steam distilled: B. distillation speed: generally l0 ~ 20min, the amount of evaporation liquid amounts to 70 ~ 100mL; C. nitrogen reco