微波消解-吸附柱分离-离子色谱法测定钢样中微量硫  

Ion chromatographic determination of trace sulfur in steel with microwave digestion and adsorption column separation

作　　者：兰宇卫[1] 陆建平[1] 章张法[1] 黄元球[1] 汤艳荣[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《冶金分析》2008年第1期24-26,共3页Metallurgical Analysis

基　　金：广西大学科研基金资(X05110)

摘　　要：建立了用微波消解样品，活性氧化铝吸附柱分离，离子色谱法测定钢中微量硫的新方法。钢样经过王水／HF／H2O2溶解和微波消解，样品中的硫转变为硫酸根离子，消解液流经吸附柱，硫酸根离子与其他金属离子分离后，用离子色谱测定硫酸根。考查了淋洗液的组成、浓度及流速对分离和测定的影响。在实验条件下，方法的线性范围为0．2～100μg／mL，检出限为0．2μg／mL。用于测定标准钢样中硫的含量，平均相对标准偏差为3．3％～6．7％（n=5），适合于大批样品的测定。A novel method has been established for the determination of trace sulfur in steel by ion chromatography with microwave digestion and active alumina column separation. Sulfur in steel sample was converted into sulfate after dissolved by aqua regia/HF/H2O2 and decomposed by microwave system, and then separated with alumina column and determined by chromatography. The influences of eluent components, concentration and flow rate on the separation and determination were studied. Under the optimized condition, the dynamic linearity located between 0. 2-100 μg/mL, and the detection limit was 0.2 μg/mL. The proposed method has been applied to the determination of sulfur in CRMs with the RSD of 3. 3%-6. 7% （n =5）. It can be widely used for the determination of sulfur in a large quantity of samples.

关 键 词：微波消解 吸附柱分离 离子色谱 钢样 硫 

分 类 号：TG115.3[金属学及工艺—物理冶金]