YS/T 896-2013Methods for chemical analysis of high purity niobium. Determination of trace impurity element content. Inductively coupled plasma mass spectrometry (English PDF)

1 Scope

This Standard stipulates the method for the determination of lithium, beryllium, boron, magnesium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, gallium, arsenic, strontium, zirconium, tantalum, molybdenum, cadmium, tin, antimony, hafnium, tungsten, lead and bismuth in high purity niobium.

This Standard is applicable to the determination of trace impurity element content in high purity niobium. The determination range is 0.0001% ~ 0.010%.

2 Method Summary

Use nitric acid and hydrofluoric acid to dissolve the test portion, use rhodium internal standard for calibration, and conduct direct determination through an inductively coupled plasma mass spectrometer. In accordance with the working curve method, calculate the mass concentration of each element, and express the determination result as mass fractions.

3 Reagents

Unless otherwise stated, the reagents used in the analysis are guaranteed reagents; the water used is Grade-1 water.

3.1 Hydrofluoric acid (rho = 1.16 g/mL).

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

3.3 Nitric acid (1 + 1).

3.4 Lithium, beryllium, boron, magnesium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, gallium, arsenic, strontium, zirconium, tantalum, molybdenum, cadmium, tin, antimony, hafnium, tungsten, lead, bismuth and rhodium single-element standard storage solution (national standard sample / national reference substance), the mass concentration is

1,000 µg/mL.

3.5 Mixed standard solution A. respectively transfer-take 10.00 mL of each element of standard storage solution (except rhodium) (3.4) in 1,000 mL plastic volumetric flasks, add 2 mL of hydrofluoric acid (3.1) and 20 mL of nitric acid (3.3); use water to dilute to the scale and mix

5 Specimens

The specimens are processed into chips with a side length not exceeding 2 mm.

6 Analytical Procedures