摘要
碳对铁硅硼非晶合金薄带的性能有重要影响。讨论了高频感应燃烧红外吸收法测定铁硅硼非晶合金薄带中碳含量的方法,优化了样品尺寸、称样量、助熔剂等关键参数。确定的最佳工作条件如下:将铁硅硼非晶合金薄带剪切为尺寸不大于5mm×5mm的碎片;称取0.2g样品于陶瓷坩埚中,按照0.2g锡-0.4g铁-1.7g钨,或0.2g锡-1.7g钨的顺序加入多元混合助熔剂;采用钢铁标准样品校准仪器。结果表明:样品尺寸对测定结果有显著影响,较大的样品尺寸会导致测定值偏低;称样量,助熔剂种类、用量及加入顺序对测定结果有轻微影响。采用0.2g锡-0.4g铁-1.7g钨作助熔剂时,方法空白值为(22±9.7)μg/g(n=10),检出限为0.003%,定量限为0.010%。采用0.2g锡-1.7g钨作助熔剂时,方法空白值为(4.4±6.7)μg/g(n=10),检出限为0.002%,定量限为0.007%。综上,实验方法的定量限为0.007%~0.010%。将实验方法用于铁硅硼非晶合金薄带实际样品分析,结果的相对标准偏差(RSD,n=8)小于3.5%,加标回收率为90%~107%。
Carbon has an important effect on the properties of iron-silicon-boron amorphous alloy strip.The determination of carbon content in iron-silicon-boron amorphous alloy strip by the high frequency induction combustion infrared absorption method was studied.The key parameters such as sample size,sample mass and flux were optimized.The optimum experimental conditions were obtained as follows:the iron-silicon-boron amorphous alloy strip sample was cut in chips with size less than 5mm×5mm;0.2g of sample was weighed and transferred into ceramic crucible,then multiple fluxes were added(0.2g of tin-0.4g of iron-1.7g of tungsten,or 0.2g of tin-1.7g of tungsten);the instrument was calibrated using certified reference materials of steel.The results showed that the sample size had a significant effect on the analysis results,and larger sample size would lead to lower determination values.The sample mass,as well as the type,dosage and addition sequence of flux had a slight effect on the analysis results.When 0.2g of tin-0.4g of iron-1.7g of tungsten were used as flux,the blank value of method was(22±9.7)μg/g(n=10).The limit of detection was 0.003%,and the limit of quantification was 0.010%.When 0.2g of tin-1.7g of tungsten were used as flux,the blank value of method was(4.4±6.7)μg/g(n=10).The limit of detection was 0.002%,and the limit of quantitation was 0.007%.Therefore,the limit of quantitation of method was 0.007%-0.010%.The proposed method was applied for the analysis of iron-silicon-boron amorphous alloy strip actual sample.The relative standard deviations(RSD,n=8)of determination results were less than 3.5%.The spiked recoveries were between 90%and 107%.
作者
刘攀
张毅
常国梁
张欣耀
LIU Pan;ZHANG Yi;CHANG Guo-liang;ZHANG Xin-yao(Luoyang Ship Material Research Institute, Luoyang 471023, China;Henan Key Laboratory of Technology andApplication of Structural Materials for Ship and Marine Equipment, Luoyang 471023, China)
出处
《冶金分析》
CAS
北大核心
2020年第9期24-30,共7页
Metallurgical Analysis
关键词
铁硅硼
非晶合金
薄带
碳
高频感应燃烧
红外吸收法
样品尺寸
iron-silicon-boron
amorphous alloy
strip
carbon
high frequency induction combustion
infrared absorption method
sample size
