氮化硼粉末中氮含量的测定
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摘要
氮化硼以其优越的机械、物理以及化学性能而得到广泛的应用,国内外市场需求也有所扩大,对氮化硼品质的要求越来越高,氮化硼中各元素的检测需求因此也更加迫切。文章采用脉冲加热惰气熔融-热导法测定氮化硼粉末中氮的含量,对分析功率、助熔剂、载气、称样量、加热时间等分析条件进行了研究,在称样量为0.02g左右,用氮化硼标准样品绘制工作曲线,用锡囊和镍蓝做为助熔剂,分析功率为6.5kW的条件下,建立了用脉冲加热惰气熔融-热导法测定氮化硼粉末中氮含量的检测方法。对氮化硼粉末样品中的氮进行了12次测定,其测定结果的相对标准偏差为1.22%,这个结果已经得到广大用户的认可,完全能够满足生产检测需求。
As boron nitride has been widely used due to its superior mechanical,physical and chemical properties,its market demands has also been expanded.With the increasingly higher requirements on the quality of boron nitride,the demands on analyzing various elements in boron nitride are more urgent.In this paper,the content of nitrogen in boron nitride powder was determined by pulsed heating inert gas and melting-thermal conductivity method.The analysis conditions of power,flux,carrier gas,sample quantity,heating time,etc.were studied.With the standard boron nitride sample being applied to draw the working curve and tin capsule and nickel blue being the flux,a method of testing nitrogen contents in boron nitride powders by pulsed inert gas melting-thermal conductivity was given with the heating power of 6.5kW.The nitrogen in boron nitride powder samples had been measured 12 times,and the relative standard deviation of the determination results was 1.22,which were accepted by the majority of users and fully met the testing demand for production.
As boron nitride has been widely used due to its superior mechanical,physical and chemical properties,its market demands has also been expanded.With the increasingly higher requirements on the quality of boron nitride,the demands on analyzing various elements in boron nitride are more urgent.In this paper,the content of nitrogen in boron nitride powder was determined by pulsed heating inert gas and melting-thermal conductivity method.The analysis conditions of power,flux,carrier gas,sample quantity,heating time,etc.were studied.With the standard boron nitride sample being applied to draw the working curve and tin capsule and nickel blue being the flux,a method of testing nitrogen contents in boron nitride powders by pulsed inert gas melting-thermal conductivity was given with the heating power of 6.5kW.The nitrogen in boron nitride powder samples had been measured 12 times,and the relative standard deviation of the determination results was 1.22,which were accepted by the majority of users and fully met the testing demand for production.
引文
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[5]卞敏,李英秋,武红英.脉冲熔融热导法测定钒粉中氮含量的不确定度评定[J].分析实验室,2008.22.
[6]于燕鹏,胡少成,马红权,等.脉冲熔融-红外吸收热导法测定钢铁材料中氧氮和氢[J].冶金分析,2014(10).
[2]杨起.氮化硼材料的性能、应用及其分析方法[J].航空维修与工程,2015(8):80-83.
[3]张相法,位星.国内外立方氮化硼进展[J].超硬材料工程,2016,28(3):3.
[4]武丽艳,郑冀腾,吴勇,等.凯氏定氮装置的改进[J].化学通报,2007(7).
[5]卞敏,李英秋,武红英.脉冲熔融热导法测定钒粉中氮含量的不确定度评定[J].分析实验室,2008.22.
[6]于燕鹏,胡少成,马红权,等.脉冲熔融-红外吸收热导法测定钢铁材料中氧氮和氢[J].冶金分析,2014(10).
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