GB/T 6609.19-2018Chemical analysis methods and determination of physical performance of alumina—Part 19: Determination of lithium oxide content—Flame atomic absorption spectrometry method (English PDF)

Foreword

GB/T 6609 "Alumina chemical analysis method and physical property determination method" is divided into 37 parts.

---Part 1. Determination of trace element content by inductively coupled plasma atomic emission spectrometry;

--- Part 2. Determination of mass loss at 300 ° C and 1000 ° C;

--- Part 3. Determination of silica content by molybdenum blue light method;

--- Part 4. Determination of ferric oxide content by o-phenanthroline spectrophotometry;

---Part 5. Determination of sodium oxide content;

---Part 6. Determination of potassium oxide content;

--- Part 7. Determination of titanium dioxide content by diantipyrylmethane photometric method;

---Part 8. Diphenylcarbazide photometric method for the determination of chromium oxide;

--- Part 9. Determination of copper oxide content by Xinyatongling spectrophotometry;

---Part 10. Benzoylphenylhydroxylamine extraction spectrophotometric determination of vanadium pentoxide content;

--- Part 11. Determination of manganese monoxide content by flame atomic absorption spectrometry;

--- Part 12. Determination of zinc oxide content by flame atomic absorption spectrometry;

--- Part 13. Determination of calcium oxide content by flame atomic absorption spectrometry;

--- Part 14. Determination of fluorine content by spectrophotometric method with ruthenium-purine complex ketone;

---Part 15. Determination of chlorine content by iron thiocyanate spectrophotometry;

---Part 16. Determination of boron trioxide content by curcumin spectrophotometry;

--- Part 17. Determination of phosphorus pentoxide content by molybdenum blue spectrophotometry;

---Part 18. Determination of sulfate content by N,N-dimethyl-p-phenylenediamine spectrophotometric method;

---Part 19. Determination of lithium oxide content by flame atomic absorption spectrometry;

---Part 20. Determination of magnesium oxide content by flame atomic absorption spectrometry;

--- Part 21. butyl rhodamine B spectrophotometric determination of gallium trioxide content;

--- Part 22. Sampling;

---Part 23. Preparation and storage of samples;

--- Part 24. Determination of the angle of repose;

---Part 25. Determination of bulk density;

---Part 26. Determination of effective density pycnometer method;

--- Part 27. Particle size analysis screening method;

---Part 28. Determination of particle size distribution of fine powders of less than 60 µm;

---Part 29. Determination of adsorption index;

--- Part 30. Determination of trace element content by X-ray fluorescence spectrometry;

--- Part 31. Determination of flow angle;

--- Part 32. Determination of alpha-aluminum oxide content - X-ray di

--- Part 33. Determination of wear index;

--- Part 34. Calculation of the content of aluminum oxide;

---Part 35. Determination of specific surface area;

--- Part 36. Determination of flow time;

--- Part 37. Determination of particle size of less than 20 µm.

This part is the 19th part of GB/T 6609.

This part is drafted in accordance with the rules given in GB/T 1.1-2009.

This part is for GB/T 6609.19-2004 "Alumina chemical analysis method and physical property determination method flame atomic absorption spectrometry Revision of the method for determining lithium oxide content. This section is compared with GB/T 6609.19-2004, except for editorial changes, major technical changes as follows.

--- Modified the measurement range from 0.005% to 0.040% to 0.005% to 0.20% (see Chapter 1, 2004 edition) Chapter 1);

--- Added a PTFE seal sampler device diagram (see Appendix A);

--- Modified the test solution for the lithium oxide mass fraction of 0.005% to 0.040% and >0.040% to 0.20% (see 6.4.2, 6.4.2 of the 2004 edition);

--- Modified the drawing steps of the working curve (see 6.5, 6.5 of 2004 edition);

---Modified the range of precision, from 0.005% to 0.040% to 0.005% to 0.20% (see Chapter 8, 2004 edition) Chapter 8).

1 Scope

This part of GB/T 6609 specifies the determination of lithium oxide content in alumina.

This section applies to the determination of lithium oxide content in alumina. Measuring range. 0.005%~0.20%.

2 Principle of the method

The sample is prepared in a sealed container of Teflon, dissolved in hydrochloric acid at a constant temperature, using an acetylene-air lean flame at the wavelength of the atomic absorption spectrometer.

The absorbance was measured at 670.8 nm to calculate the amount of lithium oxide. Equal amounts of aluminum and sodium were added to the series of standard solutions to counteract their effects.

3 Reagents and materials

Unless otherwise stated, only reagents and secondary waters identified as superior grades were used in the analysis.

3.1 aluminum, w (Al) >= 99.99%, pre-washed with a small amount of nitric acid, and then washed with water to remove nitric acid, washed twice with absolute ethanol or acetone, Dry.

3.2 Hydrochloric acid (rho=1.19g/mL).

3.3 Hydrochloric acid (1 1).

3.4 Sodium solution. Weigh 1.8859g sodium chloride (reference reagent), dissolve in water, transfer to 1000mL volumetric flask, dilute to the mark with water. Mix and store in a polyethylene bottle. 1 mL of this solution contained 1 mg of sodium oxide.

3.5 Aluminum matrix solution. Weigh 10.5853g aluminum (3.1) in a 1000mL beaker, add 240mL hydrochloric acid (3.2), to react violently After stopping, the beaker was placed on a hot plate and slowly heated until completely dissolved and cooled. Transfer the solution to a 500 mL volumetric flask and dilute with water until Scale and mix. 1 mL of this solution contained 40 mg of alumina.

3.6 Lithium oxide standard storage solution. Weigh 2.4734g and pre-dry at 280 °C ± 10 °C for 2h and cool to room temperature in a desiccator Lithium carbonate (spectral pure) was placed in a 200 mL beaker, dissolved in 20 mL of hydrochloric acid (3.3), heated to boil, cooled to room temperature, and transferred to 1000 mL. In a volumetric flask, dilute to the mark with water and mix. 1 mL of this solution contained 1 mg of lithium oxide.

3.7 Lithium oxide standard solution. Pipette 25.00mL lithium oxide standard storage solution (3.6) in a 1000mL volumetric flask, add 5mL salt Acid (3.3), dilute to the mark with water and mix. 1 mL of this solution contained 0.025 mg of lithium oxide. Available when used.

4 Instruments

4.1 PTFE sealed sample dissolver, device diagram see Appendix A.

4.2 Oven, rated temperature is not less than 350 ° C, temperature control accuracy ± 3 ° C.

4.3 Dryer, using fresh activated alumina as a desiccant.

4.4 Atomic absorption spectrometer with lithium hollow cathode lamp. Under the best working conditions of the instrument, the atomic absorption spectrometer that meets the following indicators Can be used.