GB/T 6609.12-2018Chemical analysis methods and determination of physical performance of alumina—Part 12: Determination of zinc 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 12th 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 6609.12-2004 "Alumina chemical analysis method and physical properties determination method flame atomic absorption spectrometry Revision of the method for determining zinc oxide content. This section is compared with GB/T 6609.12-2004, except for editorial changes, major technical changes as follows.

--- Modified the measurement range from "0.0004%~0.0200%" to "0.0010%~0.040%" (see Chapter 1, 2004) Chapter 1 of the edition);

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

--- Added Table 1, test procedure for zinc oxide mass fraction "0.0010%~0.010%" and " >0.010%~0.040%" (see 6.4.1);

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

--- Revised the range of precision, from "0.0004% ~ 0.0200%" to "0.0010% ~ 0.040%" (see Chapter 8, 2004 edition) Chapter 8).

1 Scope

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

This section applies to the determination of zinc oxide content in alumina. Measuring range. 0.0010%~0.040%.

2 Principle of the method

The sample was dissolved in a sealed container with hydrochloric acid at a constant temperature, and measured at an atomic absorption spectrometer wavelength of 213.3 nm using an acetylene-air flame.

Its absorbance is used to calculate the amount of zinc oxide. When drawing the working curve, the interference of aluminum is eliminated by means of aluminum matrix compensation.

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 (2 1).

3.4 Aluminum matrix solution. Weigh 25.463g of aluminum (3.1) in a 1000mL beaker and add 360mL of hydrochloric acid (3.2). Place the beaker on a hot plate and slowly heat until completely dissolved. Remove the cooling, transfer the solution into a 500mL volumetric flask, dilute with water until the moment Degree, mix. 1 mL of this solution contained 0.1 g of alumina.

3.5 Zinc oxide standard storage solution. Weigh 0.1000g of zinc oxide [w(ZnO) >= 99.99%, pre-burn at 1000 °C for 1h, and dry Cool to room temperature in a desiccator, place in a 100 mL beaker, add 5.5 mL of hydrochloric acid (3.2), dissolve, and transfer to a 1000 mL volumetric flask. Dilute the water to the mark and mix. 1 mL of this solution contained 0.1 mg of zinc oxide.

3.6 Zinc Oxide Standard Solution. Pipette 50.00mL of zinc oxide standard storage solution (3.5) in a 500mL volumetric flask and dilute with water until engraved Degree, mix. 1 mL of this solution contained 0.01 mg of zinc 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 zinc hollow cathode lamp. Under the best working conditions of the instrument, the atomic absorption spectrometer that meets the following indicators Can be used.

--- Characteristic concentration. in the solution consistent with the measurement solution matrix, the characteristic concentration of zinc oxide should be no more than 0.025µg/mL;

--- Precision. 10 times absorbance measured with the highest concentration of standard solution, the standard deviation should not exceed 1.0% of the average absorbance;