GB/T 6730.87-2023 in English
VALIDIron ores―Determination of total iron and other multi-element content―Wavelength dispersive X-ray fluorescence spectrometry (cobalt internal standard method)
- Issued on:2023-08-06
- Implemented on:2024-03-01
- File Format:PDF
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《GB/T 6730.87-2023铁矿石 全铁及其他多元素含量的测定 波长色散X射线荧光光谱法(钴内标法)》由TC317(全国铁矿石与直接还原铁标准化技术委员会)归口,主管部门为中国钢铁工业协会。
Introduction
Analysis of the core technology of standard
| Technical elements | Innovation points | Comparison with traditional methods |
|---|---|---|
| Cobalt internal standard method | Using Co₂O₃ as the internal standard to correct the matrix effect | The accuracy is improved by 30% compared with the traditional external standard method |
| Melting sample preparation | 4 fusion methods are optional (Clause 8.3-8.6) | Eliminate mineral effect and reduce the detection limit by 1 order of magnitude |
| Synchronous detection of multiple elements | 16 elements measured at one time (TFe, Si, Al, etc.) | Analysis efficiency increased by 5-8 times |
Key operating points
Glass sheet preparation specifications
The standard stipulates that the sample volume is 0.4-0.8g, the flux ratio is 10-15 times, and the amount of cobalt trioxide added is 0.1-0.2g (accuracy ±0.2mg). The melting temperature is strictly controlled in the range of 1040-1100℃, and a platinum-gold alloy (95:5) crucible is used to avoid element contamination.
Instrument parameter optimization
It is recommended to use LiF200 crystal to measure FeKβ line (tube voltage 40kV, tube current 60mA), and PET crystal to measure SiKα line. Pay special attention to the spectral interference of Br on Al (Article 5.22), which requires mathematical correction.
Quality Control System
Precision requirement: When TFe is in the range of 38-73%, the repeatability limit is r=0.5911-0.001528m (m is the average value). Use formula (3) to correct the cobalt content:
w₄=w₂-w₃×(m₅/m₆)/100
Where w₃ is the Co₂O₃ content, and m₅/m₆ is the mass ratio of the sample to cobalt.
Comparison of Standard Evolution
| Version | Detection Elements | Technical Features |
|---|---|---|
| 1986 Edition | Single Element Determination | Mainly Chemical Wet Method |
| 2023 Edition | 16 Elements Simultaneous | XRF+Cobalt Internal Standard Method |
Implementation Recommendations
- The laboratory needs to be equipped with a wavelength dispersive X-ray fluorescence spectrometer (in accordance with JJG 810) and a platinum crucible
- It is recommended to establish a calibration curve with more than 5 points, including high and low concentration standard samples
- Perform instrument drift correction every 4 hours (Formula 4-5)
- Abnormal data needs to be reviewed according to the flowchart in Appendix B

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