GB/T 4325.5-2013Methods for chemical analysis of molybdenum - Part 5: Determination of antimony content - Atomic fluorescence spectrometry (English PDF)

Foreword

GB/T 4325 "Methods for chemical analysis of molybdenum" consists of the following 26 parts:

- Part 1: Determination of lead content - Graphite furnace atomic absorption spectrometry;

- Part 2: Determination of cadmium content - Flame atomic absorption spectrometry;

- Part 3: Determination of bismuth content - Atomic fluorescence spectrometry;

- Part 4: Determination of tin content - Atomic fluorescence spectrometry;

- Part 5: Determination of antimony content - Atomic fluorescence spectrometry;

- Part 6: Determination of arsenic content - Atomic fluorescence spectrometry;

- Part 7: Determination of iron content - 1,10-phenanthroline spectrophotometry and inductively coupled plasma atomic emission spectrometry;

- Part 8: Determination of cobalt content - 5-Cl-PADAB spectrophotometry and flame atomic absorption spectrometry;

- Part 9: Determination of nickel content - Dimethylglyoxime spectrophotometry and flame atomic absorption spectrometry;

- Part 10: Determination of copper content - Flame atomic absorption spectrometry;

- Part 11: Determination of aluminum content - Chrome azurol S spectrophotometry and inductively coupled plasma atomic emission spectrometry;

- Part 12: Determination of silicon content - Inductively coupled plasma atomic emission spectrometry;

- Part 13: Determination of calcium content - Flame atomic absorption spectrometry;

- Part 14: Determination of magnesium content - Flame atomic absorption spectrometry;

1 Scope

This Part of GB/T 4325 specifies the method to determine antimony content in molybdenum.

This Part is applicable to the determination of antimony content in molybdenum powder, molybdenum bar, molybdenum trioxide, ammonium molybdate. The determination range is 0.0001%~0.0050%.

2 Method summary

The test material is decomposed with nitric acid and hydrochloric acid. In hydrochloric acid medium, use hydride generation-atomic fluorescence spectrometry to determine antimony content. Within a certain range, the fluorescence intensity is proportional to the content of the measured element. Adding molybdenum matrix can eliminate interference.

3 Reagents

Unless otherwise specified, the reagents used in this Part are guaranteed reagents; water used is grade two or above.

3.1 Sodium borohydride.

3.2 Sodium hydroxide.

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

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

3.5 Sulfuric acid (rho=1.84g/mL).

3.6 Hydrochloric acid (1+9).

3.7 Ammonia (1+99).

6 Analysis steps