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镍基合金中痕量铋的测定,在仪器分析中多数用石墨炉法,氢化物法进行测定.本法运用混合酸溶解镍基合金.然后运用电化学原理将铋析出于阴极,再用硝酸溶解,用原子吸收分光光度法在空气-乙炔火焰中对铋进行测定.本法可测定0.1μg·ml~(-1)的铋,铋的回收率达98%,精密度为1%,结果令人满意.1 仪器与试剂310型原子吸收分光光度计(上海分析仪器厂)铂网阴极;螺旋式阳极混合酸(氢氟酸+浓硝酸+浓盐酸=1+10+2)试剂均为分析纯2 分析方法称取10g镍基合金(含10%Co、8%Cr、6%Mo,1%Ti、6%Al和4%Ta,并在溶解前加入不同量的铋作回收试验),在铂皿中加混合酸10ml,加热溶解后再加H_2SO_4(1+1)20ml,用水稀释至约300ml,加入二盐酸肼8g以分解铋的络合物,制成溶液A,再配制两个含铜的溶液,将3.2g高纯度紫铜溶于HNO_3(1+1)20ml中,煮沸,稀释至1L,制成溶液B.取B溶液80ml,加入浓HNO_(3)120ml及H_2SO_4(1+1)400ml.将此混合液用水稀至4L,制成溶液C.
Determination of trace amounts of bismuth in nickel-based alloys, the majority of the instrumental analysis by graphite furnace method, hydride method for the determination of mixed acid used in this law to dissolve the nickel-based alloy and then the principle of electrochemical precipitation of bismuth in the cathode, then nitric acid The atomic absorption spectrophotometry was used to determine bismuth in the air-acetylene flame.The method can be used to determine the bismuth content of 0.1μg · ml -1, the recovery rate of bismuth is 98% and the precision is 1% Satisfactory .1 instruments and reagents 310 atomic absorption spectrophotometer (Shanghai Analytical Instrument Factory) platinum mesh cathode; spiral anode mixed acid (hydrofluoric acid + concentrated nitric acid + concentrated hydrochloric acid = 1 +10 +2) reagents are Analytical purity 2 Analytical method Weigh 10g of Ni-based alloy (containing 10% Co, 8% Cr, 6% Mo, 1% Ti, 6% Al and 4% Ta and adding different amounts of bismuth for dissolution before dissolution) , In a platinum dish add mixed acid 10ml, heated to dissolve and then add H_2SO_4 (1 +1) 20ml, diluted with water to about 300ml, was added hydrazine hydrate 8g to decompose bismuth complex solution A, and then prepared two A copper-containing solution, 3.2g of high-purity copper was dissolved in HNO_3 (1 +1) 20ml, boiled, diluted to 1L, made of solution B. Take B solution 80ml, was added concentrated HNO_ (3) 120ml and H_2SO_4 +1) 400ml. Will be mixed Mixing liquid dilute to 4L, made of solution C.