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高纯钨丝、钨粉、三氧化钨、氯化钨等产品中磷砷含量极微,光谱法及一般的钼蓝法灵敏度不够。本文采用阴离子交换树脂使钨与砷磷分离,以丁基罗丹明B与磷钼蓝、砷钼蓝生成多元络合物,分光光度法测定磷砷合量,再测定磷量,两者之差值为砷含量。丁基罗丹明B与磷钼蓝形成多元络合物,摩尔吸光系数为1.72×10~5;丁基罗丹明B与砷钼蓝形成多元络合物,摩尔吸光系数为1.42×10~5。本法具有灵敏、无毒、重现性好等优点,缺点是速度稍慢。 主要试剂:氯化铵——氢氧化铵洗液:200毫升氨水,54克氯化铵,用水稀至1升。 交换柱制备:15克50～80目国产717强碱性阴离子交换树脂,浸泡于水中数小时,
Phosphorus and arsenic content in high purity tungsten wire, tungsten powder, tungsten trioxide, tungsten chloride and other products is minimal, and the sensitivity of spectrometry and the general molybdenum blue method is not enough. In this paper, anion exchange resin was used to separate tungsten from arsenic and phosphorus. Polybutadiene was synthesized with butyl rhodamine B, phosphomolybdenum blue and arsenic molybdenum blue. The amount of phosphorous and arsenic were determined by spectrophotometry. The difference between the two Value for the arsenic content. Butyl rhodamine B formed a complex with molybdenum blue, the molar absorption coefficient was 1.72 × 10 ~ 5. Butyl rhodamine B formed a complex with arsenic molybdenum blue, the molar absorption coefficient was 1.42 × 10 ~ 5. This law is sensitive, non-toxic, reproducible, and other advantages, the disadvantage is slower. Main reagents: ammonium chloride - ammonium hydroxide lotion: 200 ml of ammonia, 54 g ammonium chloride, dilute to 1 liter with water. Exchange column preparation: 15 grams of 50-80 mesh domestic 717 strong basic anion exchange resin, soaked in water for several hours,