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氧化锑是我国的重要出口商品。每年出口量大,批次多。传统的测铅方法是采用双硫腙光度法,试样溶解后要用双硫腙四氰化碳溶液萃取两次,操作繁琐,检测时间长,不适应多批次的同时测定。本文参考了文献[1,2]后,研究了用原子吸收测定氧化锑中铅的方法,采用该方法进行回收试验,精密度试验,对照试验都取得了令人满意的结果。1 仪器与试剂 WYX—402型原子吸收分光光度计铅标准溶液:100μg·ml~(-1),称取纯铅(99.99%)0.5000g置于200ml烧杯中,加入硝酸(1+l)20ml,微热溶解,煮沸驱除氮的氧化物,冷却,移入500ml量瓶,用水稀释至刻度。2 工作曲线配制移取0.00,0.50,1.00,1.50,2.00,2.50,3.00ml铅标准溶液于100ml量瓶中加入盐酸,使溶液酸度为lmol·L~(-1)左右,用水稀释至刻度,混匀。3 分析步骤称取试样0.5000g,置于100ml高脚烧杯中,随同试样做空白试验。加入盐酸5ml,摇动试样使试样大部
Antimony oxide is an important export commodity in our country. Large volume of exports each year, many batches. The traditional method of measuring lead is to use dithizone spectrophotometric method. After the sample is dissolved, it should be extracted twice with dithizone and carbon tetracyanide solution. The operation is cumbersome and the test time is long, which is not suitable for the simultaneous determination of multiple batches. After reference [1] and [2], the method of atomic absorption spectrometry for the determination of lead in antimony oxide has been studied in this paper. The recovery test by this method has achieved satisfactory results in both the precision test and the control test. 1 instruments and reagents WYX-402 atomic absorption spectrophotometer lead standard solution: 100μg · ml -1, weighed pure lead (99.99%) 0.5000g placed 200ml beaker, add nitric acid (1 + l) 20ml , Slightly heated to dissolve, boil away nitrogen oxides, cooled, transferred to 500ml volumetric flask, diluted with water to the mark. 2 working curve preparation Pipette 0.00,0.50,1.00,1.50,2.00,2.50,3.00ml lead standard solution in 100ml volumetric flask by adding hydrochloric acid so that the solution acidity of about lmol·L ~ (-1), diluted with water to the mark, Mix well. 3 Analysis step Weigh the sample 0.5000g, placed 100ml tall feet beaker, with the sample to do a blank test. Hydrochloric acid 5ml, shake the sample to make most of the sample