GB/T 15076.15-2026Methods for chemical analysis of tantalum and niobium - Part 15: Determination of hydrogen content - Pulse infrared absorption method (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part

1.Structure and Drafting Rules of Standardization Documents". Drafting. This document is Part 15 of GB/T 15076, "Chemical Analysis Methods for Tantalum and Niobium". GB/T 15076 has the following parts published.

1.Determination of Tantalum Content in Niobium by Inductively Coupled Plasma Atomic Emission Spectrometry;

2.Determination of Niobium Content in Tantalum. Inductively Coupled Plasma Atomic Emission Spectrometry and Chromatographic Gravimetric Method;

3.Determination of Copper Content by Flame Atomic Absorption Spectrometry;

4.Determination of Iron Content by 1,10-Diazophenanthroline Spectrophotometry;

5.Determination of Molybdenum and Tungsten Contents by Inductively Coupled Plasma Atomic Emission Spectrometry;

6.Determination of Silicon Content by Inductively Coupled Plasma Atomic Emission Spectrometry;

7.Determination of Phosphorus Content in Niobium 4-Methyl-Pentanone-[2] Extraction and Separation Phosphomolybdic Blue Spectrophotometry and Inductively Coupled Plasma Bulk atomic emission spectrometry;

---Determination of carbon and sulfur content;

---Determination of iron, chromium, nickel, manganese, titanium, aluminum, copper, tin, lead and zirconium content in tantalum;

10.Determination of Iron, Nickel, Chromium, Titanium, Zirconium, Aluminum and Manganese in Niobium by Direct Current Arc Atomic Emission Spectrometry;

11.Determination of Arsenic, Antimony, Lead, Tin and Bismuth Contents in Niobium by Direct Current Arc Atomic Emission Spectrometry;

---Determination of phosphorus content in tantalum;

5 Reagents and Materials

5.1 Carrier gas. Argon, with a purity (volume fraction) of not less than 99.995%.

5.2 Power gas. Argon or nitrogen, with a purity (volume fraction) of not less than 99.9%.

5.3 Nickel flux. high-purity nickel foil or nickel bladder, wH<=0.0001%, nickel foil thickness not greater than 0.10mm.

5.4 Tin flux. tin flakes or tin granules, wH<=0.0001%.

5.5 High-purity graphite crucible.

5.6 Standard substances or standard samples. Appropriate standard substances should be selected. In principle, the chemical composition of the standard substances should be similar to that of the analytical samples.

6.Instruments and Equipment Inert gas molten infrared hydrogen analyzer, including electrode furnace, carrier gas purification and analytical gas flow conversion system, infrared cell detector, computer and software. Instrument control system. See Appendix A for instrument reference optimization analysis conditions.

7.1 The particle size of tantalum powder should be less than 700 µm, and the particle size of niobium powder should be less than 180 µm. Tantalum powder should be pre-dried under vacuum at 80°C~150°C for 4 hours, and then cooled... Cool to room temperature and vacuum-pack in a composite aluminum foil bag.

7.2 Remove the outer skin of the block sample, cut it from the core of the sample, and process it into particles with a mass of no more than 0.03g.

8 Test Procedure

8.1 Samples Weigh 0.08g to 0.12g of sample (Chapter 7), accurate to 0.0001g.

8.2 Parallel Tests Perform two parallel measurements and take the average value.

15 Determination of Hydrogen Content Pulse infrared absorption method

1.Scope This document describes a method for determining the hydrogen content in tantalum and niobium using pulsed infrared absorption. This document applies to the determination of hydrogen content in processed materials such as tantalum and niobium powder, ingots, and wires. Determination range (mass fraction). 0.0002%~0.10%.

3.Terms and Definitions This document does not contain any terms or definitions that need to be defined.

4.Principles The sample and flux were added to a high-purity graphite crucible and heated to melt under an inert gas (argon) protection. The hydrogen in the sample was in the form of hydrogen gas. After precipitation, hydrogen gas is oxidized to water by an oxidant, and then enters the infrared detector with the carrier gas flow. The detector outputs a signal, and the computer system determines the reaction based on the sample. The hydrogen content was calculated by mass, and the result was expressed as a mass fraction.