Abstract:At present, there is no corresponding national standard or industrial standard for the determination of nitrogen in aluminum-vanadium alloy. Consequently a method for the determination of nitrogen in aluminum-vanadium alloy by inert gas fusion-thermal conductivity was established. The optimum experimental conditions for the analysis of nitrogen were investigated. In experiments, 0.07g of sample was put into the nickel basket, which was then transferred into graphite crucible after degassing. The analysis power was controlled at 5.0kW and the analysis time of nitrogen was 60s. The instrument was calibrated using standard aluminum-vanadium alloy sample. The proposed inert gas fusion-thermal conductivity method was applicable for the determination of nitrogen content in aluminum-vanadium alloy. The limit of detection was 0.00012%. The limit of quantification was 0.0004%, which was calculated by 10 times of standard deviation of the blank. The method was adopted to determine the nitrogen content in two aluminum-vanadium alloys. The relative standard deviation (RSD, n=11) of results were between 6.9% and 11%. The spiked recoveries were between 94% and 107%.
彭倩,沈保罗.锆合金的织构及其对性能的影响[J].稀有金属,2005,29(6):414-418.PENG Qian,SHEN Bao-Luo.Texture of zirconium alloy and its effects on properties[J].Chinese Journal of Rare Metals,2005,29(6):414-418.
[2]
Winge R K,Fassel V A.Simultaneous determination of oxygen and nitrogen in refractory metals by the direct current carbon-arc,gas chromatographic technique[J].Analytical Chemistry,1965,37(1):67-70.
[3]
王宽,李波,孙宝莲,等.惰性气体中熔融试样-红外光谱法测定锡钛合金中氧含量[J].理化检验:化学分册,2014,50(6):737-739.WANG Kuan,LI Bo,SUN Bao-lian,et al.Determination of oxygen in tin titanium alloy by inert gas fusion-infrared method[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(6):737-739.
[4]
Smiley W G.Determination of oxygen in metals without high vacuum by capillary trap method[J].Analytical Chemistry,1955,27(7):1098-1102.
[5]
王宽,梁清华,周恺,等.惰气熔融-红外吸收法测定钛钼合金中氧[J].冶金分析,2015,35(3):61-63.WANG Kuan,LIANG Qing-hua,ZHOU Kai,et al.Determination of oxygen in titanium-molybdenum alloy by inert gas fusion-infrared absorption method[J].Metallurgical Analysis,2015,35(3):61-63.
[6]
Inoue R,Suito H.Determination of oxygen in iron-aluminum alloy by inert gas fusion-infrared absorptiometr[J].Materials Transactions,1991,32(12):1164-1169.
[7]
王宽,周恺,李波,等惰气熔融-红外/热导法同时测定锆合金中氧和氮[J].冶金分析,2017,37(1):81-84.WANG Kuan, ZHOU Kai,LI Bo,et al.Simultaneous determination of oxygen and nitrogen in zirconium alloy by inert gas fusion-infrared and thermal conductivity method[J].Metallurgical Analysis,2017,37(1):81-84.
[8]
程晓舫,程坚平,杨劲松.惰气熔融-热导法测定钒氮合金中氮[J].冶金分析,2004,24(2):68-69.CHENG Xiao-fang,CHENG Jian-ping,YANG Jin-song.Determination of nitrogen in vanadium-nitrogen alloy by inert gas fusion thermal conductivity method[J].Metallurgical Analysis,2004,24(2):68-69.
[9]
钟华.惰气熔融-红外吸收/热导法同时测定钒铝中间合金中氧氮[J].冶金分析,2014,34(12):7-12.ZHONG Hua.Simultaneous determination of oxygen and nitrogen invanadium-aluminum master alloy by inert gas fusion-infrared absorption/thermal conductivity method[J].Metallurgical Analysis,2014,34(12):7-12.
[10]
石新层,王辉,李波.TC-600对钛及钛合金中氧、氮的联合测定[J].钛工业进展,2007,24(3):23-25.SHI Xin-ceng,WANG Hui,LI Bo.Determining oxygen and nitrogen simultaneously in titanium and titanium alloys with TC-600 oxygen-azote determinator[J].Titanium,2007,24(3):23-25.
[11]
孙金库,秦毅,王树安.红外吸收法和热导法测定铀钼合金中氧和氮[J].冶金分析,2010,30(5):6-8.SUN Jin-ku,QIN Yi,WANG Shu-an.Determination of oxygen and nitrogen in U-Mo alloy by infrared absorption and thermal conductivity[J].Metallurgical Analysis,2010,30(5):6-8.
[12]
周海收,王启芳.稀土金属钕和镝中氧氮的测定方法研究[J].分析试验室,2005,24(3):79-81.ZHOU Hai-shou,WANG Qi-fang.Determination of oxygen and nitrogen in the metals of neodymium and dysprosium[J].Chinese Journal of Analysis Laboratory,2005,24(3):79-81.
[13]
Banks C V,O'Laughlin J W,Kamin G J.Determination of oxygen in yttrium and yttrium fluoride by the inert gas fusion method[J].Analytical Chemistry,1960,32(12):1613-1616.
[14]
高光洁子,冯圣雅,王莘泉,等.惰气熔融-脉冲加热法同时测定NdFeB合金中氧和氮[J].冶金分析,2011,31(1):30-34.GAO Guang-jie-zi,FENG Sheng-ya,WANG Xin-quan,et al.Simultaneous determination of oxygen and nitrogen in NdFeB alloy by inert gas fusion impulse heating method[J].Metallurgical Analysis,2011,31(1):30-34.