GB/T 6150.17-2022

Methods for chemical analysis of tungsten concentrates—Part 17：Determination of antimony content—Atomic fluorescence spectrometry (English Version)

Standard No.

GB/T 6150.17-2022

Language

Chinese, Available in English version

Release Date

2022

Published By

General Administration of Quality Supervision, Inspection and Quarantine of the People‘s Republic of China

Latest

GB/T 6150.17-2022

Replace

GB/T 6150.17-2008

Scope

This document specifies the method for the determination of antimony content in tungsten concentrates. This document is applicable to the determination of antimony content in tungsten concentrate, the determination range (mass fraction): 0.0010% ~ 0.20%.

Introduction

Analysis of core changes in standards

Technical indicators	GB/T6150.17-2008	GB/T6150.17-2022	Upgrade benefits
Detection method	Hydride atomic absorption spectrometry	Atomic fluorescence spectrometry	Detection limit reduced from 0.002% to 0.001%
Precision control	Allowable difference management	Systematic reproducibility indicators	Meet ISO17025 certification requirements

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Key instrument technical specifications

The atomic fluorescence spectrometer used must meet the following requirements:

• Detection limit:≤1ng/mL
• Curve linearity:R²≥0.90
• Environmental adaptability:Acid and alkali gas corrosion resistant design

With antimony special cathode lamp, the signal-to-noise ratio is optimized to 10^-4 μg/L.

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Precision control requirements

Antimony content range (%)	Repeatability limit (r)	Reproducibility limit (R)
0.0010-0.008	±0.0013	±0.0025
0.04-0.06	±0.005	±0.011

Note: The inter-laboratory comparison data comes from 72 hours of continuous testing by 8 authoritative institutions

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Highlights of test process optimization

1. Pretreatment speed-up: The sulfuric acid-ammonium sulfate mixed system is used to shorten the sample decomposition time by 35%
2. Interference treatment: The citric acid complexation combined with thiourea system improves the efficiency of removing iron and manganese interference by 60%

Application verification case

A testing room tested the 0.15% antimony standard sample 10 times in a row:

• Range value <0.02% (MAS limit 0.03%)
• RSD<0.8% (better than the international EP specification 1.5%)

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New standard practice guidance

Implementation phase	Key control points
Laboratory modification	Need to be equipped with silicon carbide heating module for heating digestion device
Staff training	Focus on the control of hydride formation under non-equilibrium conditions