样品制备对金属中微量氧、氮、氢分析结果的影响

Effect of sample treatment on determination results of micro amounts of oxygen,nitrogen and hydrogen in metals

应用氧氮测定仪、氢测定仪和氧氮氢分析仪,完成高纯金属和高温合金等金属材料中微量氧氮氢的测定,并考察了样品制备对分析结果的影响。结果表明,样品制备方式直接影响微量氧、氮、氢分析结果的准确性。对于炉前用石英玻璃管快淬直接成型并低温保存在液氮罐中钢试样,用快速车制的方式制样测得氢的结果要比直接切断或慢速车制的方式明显偏低;对于表面光洁已用四氯化碳去油,但未经酸洗的纯镍试样,其氧,氮,氢的测定值比经酸处样试样的测定值高,其中氧含量约高4倍。因此,在制备样品时要选择恰当制样方法。通过控制好空白值、分析参数、标准参考物质、样品制备四个要素,成功地测定了金属中微量氧、氮、氢含量。

Determination of micro amounts of oxygen, nitrogen and hydrogen in high-pure metals and superalloy is performed by nitrogen/oxygen determinator, hydrogen determinator and hydrogen/nitrogen/oxygen analyzer. The effect of surface treatment of samples on the hydrogen, nitrogen and oxygen analysis results is investigated. It is shown that the treatment affects the accuracy of the determination. For the steel sample quenched in cool water within the quartz pipes and put in liquid nitrogen, the rapid turning of sample gives evidently lower result of hydrogen than direct cutting or slow turning of one. For the pure nickel sample possessed of brigh color surface and cleaned with CCl4, the determination value of unpickled sample is larger than that of pickled one for hydrogen, nitrogen and oxygen. Therein, oxygen content of the unpickled one is five times that of the pickled one. It is very important for microanalysis to select the suitable methods of sample preparation. The microanalysis of hydrogen, nitrogen and oxygen in metals has been done well by controlling blank, analysis parameter, standard reference material and sample treatment.