YS/T 63.16-2019 in English

Standard Update and Technological Evolution

As the 16th part of the YS/T 63 series of standards, YS/T 63.16-2019 focuses on regulating the application of wavelength dispersive X-ray fluorescence spectrometer in the element detection of carbon materials for aluminum. Compared with the 2006 version of the standard, the main technical improvements are reflected in:

Analysis of core detection technology

Principle of X-ray fluorescence

When the primary X-ray emitted by the end window Rh target X-ray tube irradiates the sample, the inner electrons of each element atom are excited, generating secondary characteristic X-rays of specific wavelengths. Element analysis is completed by measuring the wavelength (qualitative) and intensity (quantitative) of these characteristic spectral lines in combination with the calibration curve.

Key instrument configuration

• Spectrometer resolution: LiF200 crystal is required for spectroscopy, and PET crystal is required for light element measurement
• Sample preparation system: Tungsten carbide mortar + 20kN tablet press, ensuring that the sample density is ≥4mm
• Environmental control: Constant temperature and humidity laboratory to reduce instrument drift

Operation specification and quality control

Sample preparation process

1. Sampled according to GB/T 26297.3/6, crushed to <4mm
2. Sieve through 150μm sieve and dried at 110℃ for 2h
3. Mixed and ground with stearic acid at a ratio of 6:1 for 20s
4. Pressed and molded at 20kN pressure for 20s

Calibration requirements

Implementation Suggestions

Key points for laboratory construction

It is recommended to configure a vacuum type wavelength dispersive spectrometer. When detecting light elements (S, P, etc.), the vacuum degree must be maintained at ≤10Pa. Drift correction is required with monitoring samples every day. It is recommended to use NIST standard material SRM679 (graphite) as a quality control sample.

Method verification requirements

When creating a new method, it is necessary to verify: Repeatability limit (r) ≤ 0.0005% (for S element), Detection limit ≤ 0.0003% (Fe element). It is recommended to use a spike recovery experiment to verify accuracy, and the recovery rate should be controlled at 95%-105%.