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硅的极谱测定有间接法,直接法与伏安法等。我们研究了在一定条件下使SiO_4~(2-)与MoO_4~(2-)形成β-12-硅钼酸。通过测定硅钼酸中组成钼的催化波来间接测定硅,灵敏度为7×10~(-10)M(0.02ppb)。本法应用于高纯铟中痕量硅的测定,可检测至4×10~(-6)％。实验仪器与试剂:8960型极谱仪(上海冶金所,上海分析仪器厂)。反渗透水;各种酸均为MOS级或亚沸蒸馏;钼酸铵(E.Merck,G.R);试样表面腐蚀剂为醋酸-硝酸-氢氟酸(5:15:2);极谱底液为2.5％氯酸钾-0.1M苯羟乙酸-0.5M硫酸。
Polarographic determination of silicon indirect method, direct method and voltammetry and so on. We have studied the formation of β-12-silico-molybdic acid from SiO_4 ~ (2-) and MoO_4 ~ (2-) under certain conditions. The indirect determination of silicon by measuring the catalytic wave of molybdenum in molybdosilicic acid has a sensitivity of 7 × 10 -10 M (0.02 ppb). This method is applied to the determination of trace silicon in high purity indium and can detect up to 4 × 10 -6%. Experimental equipment and reagents: 8960-type polarography (Shanghai Metallurgical Institute, Shanghai Analytical Instrument Factory). Reverse osmosis water; various acids are MOS-grade or sub-boiling distillation; ammonium molybdate (E. Merck, GR); sample surface etchant is acetic acid - nitric acid - hydrofluoric acid The liquid is 2.5% potassium chlorate -0.1M benzilic acid - 0.5M sulfuric acid.