Plotnikov Alexei, Pfeifer Jens, Richter Silke, Kipphardt Heinrich, Hoffmann Volker
BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489, Berlin, Germany,
Anal Bioanal Chem. 2014 Nov;406(29):7463-71. doi: 10.1007/s00216-014-8185-x. Epub 2014 Oct 12.
Fast flow glow discharge mass spectrometry with a Grimm-type ion source providing a high sputter rate was used for the determination of major nonmetallic impurities in magnesium. The analytical signal was found to be strongly influenced by the electrical discharge parameters. For calibration by standard addition, synthetic standard samples were produced in two different ways-namely, by pressing and by sintering doped metal powders. The observed sensitivity of the calibration curves was shown to depend on the particle size of the powder. For the magnesium powders, the mass fractions of oxygen, nitrogen, boron, and silicon were determined to be about 0.01 kg·kg(-1) (relative standard deviation approximately 10-20 %), 2,700 mg·kg(-1), 150 mg·kg(-1), and 300 mg·kg(-1), respectively.
采用具有高溅射速率的格林姆型离子源的快速流动辉光放电质谱法测定镁中的主要非金属杂质。发现分析信号受放电参数的强烈影响。为了通过标准加入法进行校准，以两种不同方式制备合成标准样品，即压制和烧结掺杂金属粉末。结果表明，校准曲线的观测灵敏度取决于粉末的粒径。对于镁粉，测定的氧、氮、硼和硅的质量分数分别约为0.01 kg·kg⁻¹（相对标准偏差约为10 - 20%）、2700 mg·kg⁻¹、150 mg·kg⁻¹和300 mg·kg⁻¹。
