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取尿2.5毫升放10毫升烧杯内,加2:5(V/V)硫酸硝酸混合液0.5毫升及2滴高氯酸,盖以合适的称量瓶盖。放电炉上用调压变压器控制加热消化至无色透明,取下冷却后再加1滴高氯酸重加热至冒烟不烧干,冷却后加少量重蒸水敞口蒸至近干取下,加2.5毫升底液(配制:取1％抗坏血酸60毫升,10％酒石酸20毫升,10％碘化钾20毫升,0.1％聚乙烯醇2毫升,加水至200毫升)。用JP-1A示波极谱测定:三电极,导数,原点电位-0.40～-0.45伏(对SCE),“电流倍率”0.004～0.01,峰电位在-0.50～-0.56伏。用标准加入法计算含量。
Take 2.5 ml of urine into a 10 ml beaker and add 0.5 ml of 2: 5 (v / v) sulfuric acid and nitric acid mixture and 2 drops of perchloric acid and cover with a suitable weighing bottle cap. Discharge furnace with a voltage regulating transformer control heating and digestion to colorless and transparent, remove the cooling and then add a drop of perchloric acid heavy heating to smoke does not burn, add a small amount of steam after cooling and steaming to near dry, Add 2.5 ml of the bottom liquid (preparation: take 1% ascorbic acid 60 ml, 10% tartaric acid 20 ml, 10% potassium iodide 20 ml, 0.1% polyvinyl alcohol 2 ml, add water to 200 ml). With the oscillopolarographic determination of JP-1A: three electrodes, derivative, the origin potential of -0.40 ~ -0.45 volts (for SCE), “current ratio” 0.004 to 0.01, the peak potential of -0.50 ~ -0.56 volts. Use standard addition method to calculate the content.