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提出硫化铵溶解,氨性介质过氧化氢氧化分解硫磺试样,在0.48mol·L~(-1)HClO_4-4.76×10~(-3)mol·L~(-1)Na_2SO_3-2.96mol·L~(-1)NH_3·H_2O-6.81×10~(-3)mol·L~(-1)(NH_4)_2SO_4-8.41×10~(-4)mol·L~(-1)KIO_3-1.18×10~(-2)mol·L~(-1)硫脲-0.02g·L~(-1)动物胶体系中以催化极谱法测定痕量硒的方法.硒浓度在0.02～9.0ng·ml~(-1)范围内与极谱峰电流有良好的分段线性关系,检出限为0.01ng·ml~(-1).方法的RSD为3.4%～3.9%,加标回收率为91%～97%.此法仪器试剂简单,操作快速简便.用于硫磺样品的测定,结果满意.
Ammonium sulphide dissolution and ammoniacal hydrogen peroxide oxidative decomposition of sulfur samples were proposed. Under the conditions of 0.48 mol·L -1 HClO 4 -4.76 × 10 -3 mol·L -1 Na 2 SO 3 -2.96 mol·L -1 L ~ (-1) NH_3 · H_2O-6.81 × 10 ~ (-3) mol·L ~ (-1) (NH_4) _2SO_4-8.41 × 10 ~ (-4) mol·L -1 KIO_3-1.18 × 10 ~ (-2) mol·L -1 Thiourea -0.02g · L -1 Animal glue system Determination of trace selenium by catalytic polarography Selenium concentration of 0.02 ~ 9.0ng · The range of ml ~ (-1) showed a good linear relationship with polarographic peak current, with a detection limit of 0.01 ng · ml -1 .The RSD of the method was 3.4% -3.9% 91% ~ 97% .The method reagent is simple, the operation is quick and easy.It is used for the determination of sulfur sample with satisfactory results.