YS/T 273.14-2008Chemical analysis methods and determination of physical performance of synthetic cryolite. Part 14: X-ray fluorescence spectrometric method for the determination of elements content (English PDF)

Foreword

YS/T 273 "cryolite chemical analysis methods and determination of physical performance" is divided into 14 parts.

--- Part 1. Determination of the content of water in wet weight method;

--- Part 2. Determination of burning reductions;

--- Part 3. distillation - thorium nitrate volumetric method for the determination of fluorine content;

--- Part 4. Determination of aluminum content - EDTA volumetric method;

--- Part 5. Determination by flame atomic absorption spectrometry sodium content;

--- Part 6. molybdenum blue spectrophotometric determination of silicon dioxide content;

--- Part 7. phenanthroline spectrophotometric determination of ferric oxide content;

--- Part 8. Determination of sulfate content barium sulphate gravimetric method;

--- Part 9. molybdenum blue spectrophotometric determination of phosphorus pentoxide content;

--- Part 10. Determination of free weight alumina content;

--- Part 11. Determination of the sulfur content of X-ray fluorescence spectrometry;

--- Part 12. Flame atomic absorption spectrometric method for the determination of calcium oxide content;

--- Part 13. sample preparation and storage;

--- Part 14. Determination of Elements in X-ray fluorescence spectroscopy.

This is Part 14.

Appendix A of this section is an informative annex.

The non-ferrous metal part by the National Standardization Technical Committee and centralized.

This part of the Aluminum Corporation of China Zhengzhou Research Institute, China Nonferrous Metals Industry Institute of Standards Metrology and Quality is responsible for drafting.

This section is more fluoride Chemical Co., Ltd., Neimengguhuo coal Hongjun Aluminum Co., Ltd., Fujian Nanping Aluminium Company Limited Division participated in the drafting.

1 Scope

This section provides cryolite fluorine, aluminum, sodium, silicon, iron, sulfur, phosphorus, calcium content (F, Al, Na, SiO2, Fe2O3, SO2-4, P2O5, CaO represented) measurement method.

This section applies to the determination of fluorine in cryolite, aluminum, sodium, silicon, iron, sulfur, phosphorus, calcium content. Determination of the range in Table 1.

Table 1

Component measuring range /% F 40.00 ~ 60.00 Al 11.00 ~ 18.00 Na 20.00 ~ 35.00 SiO2 0.010 ~ 0.60 Component measuring range /% Fe2O3 0.010 ~ 0.50 SO2-4 0.10 ~ 2.00 P2O5 0.0010 ~ 0.30 CaO 0.0060 ~ 1.00

2 Principle of the method

Mixing the molten sample flux anhydrous lithium tetraborate and lithium metaborate, plus a small amount of lithium bromide (or iodide) as a release agent. In the melt prototype Melted into glass samples. Measured by X-ray fluorescence spectrometer. Theoretical coefficient alpha or fundamental parameter calibration between the absorbent element -Enhancement.

3 Reagents

3.1 anhydrous lithium tetraborate and lithium metaborate mixed flux [Li2B4O7 (67%) + LiBO2 (33%)]. at 700 °C burning 2h, dry place Dryer saved.

3.2 remover. a saturated solution of lithium bromide or ammonium iodide solution (300g/L).

3.3 Sample Monitoring. Monitor sample should be stable glass, contains all the elements of calibration, so that its content should be less than the statistical error count rate or equal to the count rate calibration element statistical error.

4 Instrument

Platinum 4.1 - gold alloy crucible (95% Pt + 5% Au).

4.2 platinum - gold alloy casting (95% Pt + 5% Au). bottom mold material thickness of about 1mm, making it difficult to deformation.

Note. The sample vessel melt casting mold can be combined. If the sample in the crucible directly after melt molding, the bottom surface of the inner wall of the crucible is required smooth.

4.3 fusion machine. automatic flame melt melting prototype or high-frequency inductors, if other types of prototype melting temperature not lower than 1100 °C, and can be controlled Temperature, control accuracy of ± 15 °C.

4.4 wavelength dispersive X-ray fluorescence spectrometer. end window rhodium anode X-ray tube.

5 Sample

The specimen shall conform YS/T 273.13 in 3.3 requirements.