GB/T 23524-2019Method for chemical analysis of petrochemical spent platinum catalyst—Determination of platinum—Inductively coupled plasma atomic emission spectrometry (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This standard replaces GB/T 23524-2009 "Petrochemical waste catalysts in the determination of platinum content inductively coupled plasma atomic Shot spectroscopy. Compared with GB/T 23524-2009, this standard is subject to the following technical changes as follows.

--- In the standard, the method of oxidizing complex platinum with hydrochloric acid and sodium chlorate is used to replace the chlorine gas oxidative complexing method in the original standard, and the standard is deleted. The content of chlorine gas oxidative complexation method in the full text;

--- Remove the contents of Appendix A, Appendix B is adjusted to Appendix A.

1 Scope

This standard specifies the determination method of platinum content in petrochemical aluminum-silicon carrier waste platinum catalyst.

This standard applies to the determination of platinum content in petrochemical aluminum-silicon carrier waste platinum catalyst. Measuring range. 0.100%~0.800%.

2 Method summary

Dissolve the sample with sulfuric acid, oxidize the complexed platinum with hydrochloric acid and sodium chlorate, and select the best inductively coupled plasma atomic emission spectrometer. The platinum content was determined under working conditions.

3 Reagents and materials

3.1 Unless otherwise stated, analytically pure reagents or higher purity reagents and distilled water or equivalent purity water were used in the analysis.

3.2 Sodium chlorate.

3.3 Sodium hydroxide.

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

3.5 Nitric acid (rho = 1.42 g/mL).

3.6 sodium chlorate solution (80g/L). Weigh 40g sodium chlorate (3.2), dissolved in 100mL water, transferred to a 500mL volumetric flask to determine the volume, Shake well.

3.7 Hydrochloric acid (1 1).

3.8 Sulfuric acid (1 1).

3.9 Platinum standard storage solution (1mg/mL). Weigh 1.0000g of platinum powder (wPt>=99.99%) in a 250mL beaker, add 30mL Hydrochloric acid (3.4) and 10mL nitric acid (3.5), covered with a watch glass, heated at low temperature until dissolved completely, and steamed to near dryness, taken off slightly cold, added 10mL Hydrochloric acid (3.4), evaporated to near dryness, repeat this operation 3 times, drive off the nitrogen oxides, add 40mL hydrochloric acid (3.7) to dissolve the salt at low temperature, remove the burning Cup, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, shake.

3.10 Nickel. 50mL.

3.11 Argon (mass fraction >= 99.99%).

4 Instruments

Inductively coupled plasma atomic emission spectrometer. Under the best working conditions of the instrument, anyone who can achieve the following indicators can be used.

--- Light source. Argon plasma source, the maximum output power of the generator is not less than 1.30kW.

--- Resolution. The optical resolution is not more than 0.010 nm at 200 nm; the optical resolution is not more than 0.020 nm at 400 nm.

---Instrument stability. Under the best working conditions of the instrument, the light intensity phase is measured 11 times with 1µg/mL copper standard solution. The standard deviation is not more than 2.5%.