悬浮液进样-液体阴极辉光放电原子发射光谱法测定高纯氮化硅粉体中微量杂质元素
发布时间：2018-10-09 07:39
【摘要】：针对高纯氮化硅粉体中的9种微量杂质元素(Al、Ca、Co、Fe、K、Mg、Mn、Na、Ni),建立了悬浮液进样-液体阴极辉光放电原子发射光谱定量分析方法。考察了制备稳定悬浮液对样品颗粒度的要求,并通过六通阀将悬浮液引入液体阴极辉光放电原子发射光谱装置检测。本方法采用水溶液标准进行定量分析,无需对悬浮液的p H值进行精确调节,能够保持液体阴极辉光等离子体的稳定性。研究了仪器装置的操作电压、载液流速、光电倍增管积分时间等因素对检出限的影响。优化后得到的最佳实验条件为操作电压1080 V,载液流速1.2 m L/min,光电倍增管积分时间800 ms。利用六通阀进样系统对原有的液体阴极辉光放电原子发射光谱装置进行改进,从而实现悬浮液直接进样检测。用此装置对氮化硅实际样品进行检测,得到各种元素的检出限在0.2~53 mg/kg之间,RSD在1.1%~5.0%之间。通过对氮化硅标准参考物质ERM-ED101进行分析,其测定结果与高温高压消解-电感耦合等离子体发射光谱法一致,并与标准参考值吻合,表明此方法可用于氮化硅粉体的悬浮液直接进样检测,结果准确可靠,灵敏度高,具备应用价值。
[Abstract]:Aiming at nine trace impurity elements (Al,Ca,Co,Fe,K,Mg,Mn,Na,Ni) in high purity silicon nitride powder, a quantitative analysis method of suspension injection and liquid cathode glow discharge atomic emission spectrometry was established. The requirements of preparing stable suspensions for sample size were investigated, and the suspension was introduced into liquid cathodic glow discharge atomic emission spectrometer by a six-way valve. The stability of liquid cathode glow plasma can be maintained without adjusting the pH value of suspensions accurately by using the aqueous solution standard for quantitative analysis. The effects of operating voltage, liquid velocity and integration time of photomultiplier tube on the detection limit are studied. The optimized experimental conditions are as follows: operating voltage 1080 V, liquid flow rate 1.2 mL / min, integral time of photomultiplier tube 800 ms.. The original liquid cathodic glow discharge atomic emission spectrometer was improved by using the six-way valve sampling system, so as to realize the direct sampling detection of suspensions. The detection limit of various elements was found to be between 0.2 ~ 53 mg/kg and 1.1% ~ 5.0% by using this device for the detection of silicon nitride samples. By analyzing the standard reference material (ERM-ED101) of silicon nitride, the results are in agreement with the high temperature and high pressure digestion-inductively coupled plasma emission spectrometry (ICP-AES), and the results are in good agreement with the standard reference values. The results show that this method can be used for the direct injection of silicon nitride powder suspension, the results are accurate and reliable, high sensitivity and application value.
【作者单位】： 中国科学院上海硅酸盐研究所;
【基金】：中国科学院科研装备研制项目(No.YZ201539)、中国科学院仪器设备功能开发技术创新项目(No.Y67YQ2120G) 上海市无机非金属材料分析测试表征专业技术服务平台项目(No.14DZ2292900)资助
【分类号】：O657.31;TQ127.2
本文编号：2258520
[Abstract]:Aiming at nine trace impurity elements (Al,Ca,Co,Fe,K,Mg,Mn,Na,Ni) in high purity silicon nitride powder, a quantitative analysis method of suspension injection and liquid cathode glow discharge atomic emission spectrometry was established. The requirements of preparing stable suspensions for sample size were investigated, and the suspension was introduced into liquid cathodic glow discharge atomic emission spectrometer by a six-way valve. The stability of liquid cathode glow plasma can be maintained without adjusting the pH value of suspensions accurately by using the aqueous solution standard for quantitative analysis. The effects of operating voltage, liquid velocity and integration time of photomultiplier tube on the detection limit are studied. The optimized experimental conditions are as follows: operating voltage 1080 V, liquid flow rate 1.2 mL / min, integral time of photomultiplier tube 800 ms.. The original liquid cathodic glow discharge atomic emission spectrometer was improved by using the six-way valve sampling system, so as to realize the direct sampling detection of suspensions. The detection limit of various elements was found to be between 0.2 ~ 53 mg/kg and 1.1% ~ 5.0% by using this device for the detection of silicon nitride samples. By analyzing the standard reference material (ERM-ED101) of silicon nitride, the results are in agreement with the high temperature and high pressure digestion-inductively coupled plasma emission spectrometry (ICP-AES), and the results are in good agreement with the standard reference values. The results show that this method can be used for the direct injection of silicon nitride powder suspension, the results are accurate and reliable, high sensitivity and application value.
【作者单位】： 中国科学院上海硅酸盐研究所;
【基金】：中国科学院科研装备研制项目(No.YZ201539)、中国科学院仪器设备功能开发技术创新项目(No.Y67YQ2120G) 上海市无机非金属材料分析测试表征专业技术服务平台项目(No.14DZ2292900)资助
【分类号】：O657.31;TQ127.2
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