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作 者:常国梁 刘攀[1] 张毅[1] CHANG Guo-liang;LIU Pan;ZHANG Yi(Luoyang Ship Material Research Institute, Luoyang 471023, China)
机构地区:[1]中国船舶重工集团公司第七二五研究所(洛阳船舶材料研究所),河南洛阳471023
出 处:《冶金分析》2020年第7期16-21,共6页Metallurgical Analysis
摘 要:蒙乃尔(Monel)合金是一种以镍、铜为基体成分的特种耐蚀合金,典型成分为67%Ni-30%Cu。现行标准方法GB/T 21931.1—2008《镍、镍铁和镍合金碳含量的测定高频燃烧红外吸收法》对Monel合金在内的分析条件不甚明确,且实验中存在熔融物喷溅等现象,基于此,开展了高频感应燃烧-红外吸收光谱法测定Monel合金中碳含量的方法研究。探讨了助熔剂、样品量对碳含量测定的影响,并从检出限、精密度、回收率等方面进行方法学评价,建立了适用于Monel合金中碳含量测定的专用方法。确定的最佳分析条件为:称取0.20~0.30g样品于陶瓷坩埚中,加入1.5~2.0g钨粒作助熔剂;采用钢铁标准样品校正仪器,校准曲线的线性相关系数r=0.999。方法的检出限为0.001%,定量限为0.003%。应用于Monel K500、Monel 400实际样品中碳的测定,结果的相对标准偏差(RSD,n=8)小于3%。加入钢铁标准样品进行加标回收试验,回收率为92%~106%。本法结果同GB/T 21931.1—2008一致。Monel alloy is a kind of special corrosion resistant alloy based on nickel and copper,and the typical composition is 67%Ni-30%Cu.The current standard method GB/T 21931.1-2008<Nickel,ferronickel and nickel alloys-Determination of carbon content-Infrared absorption method after induction furnace combustion>has some problems,such as unclear analysis conditions and the phenomenon of melt splash in test.Therefore,the determination method of carbon content in Monel alloy was studied by the high frequency induction combustion-infrared absorption spectroscopy was studied.The effect of flux and sample mass on the determination of carbon was investigated.The methodological evaluation was carried out from the aspects including limit of detection,precision and recovery.Then a special method suitable for the determination of carbon content in Monel alloy was established.The optimum analysis conditions were obtained as follows:0.20-0.30g of sample was weighed and transferred into ceramic crucible;1.5-2.0g of granular tungsten was added as flux;the analyzer was calibrated using certified reference material of steel;the linear correlation coefficient of the calibration curve was r=0.999.The limit of detection was 0.001%and the limit of quantification was 0.003%.The proposed method was applied to the determination of carbon in actual samples of Monel K500 and Monel 400.The relative standard deviation(RSD,n=8)of determination results was less than 3%.The recovery tests of carbon were conducted by adding certified reference material of steel.The recoveries were between 92%and 106%.The results of proposed method were consistent with GB/T 21931.1-2008.
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