Overview
ISO 13547-1:2014 - "Copper, lead, zinc and nickel sulfide concentrates - Determination of arsenic - Part 1" defines an iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric (ICP‑AES) procedure for measuring the mass fraction of arsenic in sulfide concentrates. The method covers arsenic ranges for different concentrates:
- Copper sulfide: 0.05 % to 2.0 % As
- Lead sulfide: 0.05 % to 1.0 % As
- Zinc sulfide: 0.05 % to 0.6 % As
- Nickel sulfide: 0.05 % to 1.0 % As
The procedure combines acid decomposition of a test portion, coprecipitation of arsenic with iron hydroxide to separate it from the sample matrix, and quantification by ICP‑AES using iron‑matched standards.
Key Topics and Requirements
- Principle: Acid digestion (nitric/sulfuric), coprecipitation of arsenic on iron hydroxide, measurement by ICP‑AES.
- Analytical scope: Specified As mass-fraction ranges for copper, lead, zinc and nickel sulfide concentrates.
- Reagents and purity: Use analytical‑grade reagents and high‑purity water; prepared arsenic standard solutions are specified.
- Apparatus: ICP‑AES (recommended emission wavelengths 193.696 nm or 197.197 nm), acid‑resistant PTFE beakers, specified filter papers and precision balances.
- Sampling and test portions: Laboratory and test sample preparation per ISO guidance; option to use pre‑dried test portions (Annex A).
- Procedure controls: Blank tests, duplicate determinations (repeatability), removal of interferences (e.g., lead sulfate), calibration with iron‑matched standards.
- Quality and precision: Includes precision expressions, between‑laboratory precision guidance, and trueness checks.
- Safety: Warning about hazardous materials and operations; users must implement appropriate health and safety practices.
Applications and Users
ISO 13547-1:2014 is used for reliable arsenic determination in sulfide concentrates and is relevant to:
- Metallurgical and assay laboratories performing chemical analysis of concentrates
- Mining companies and concentrator QC/QA teams monitoring arsenic content
- Smelters and metal processors assessing feedstock impurity levels
- Certification and compliance testing where accurate arsenic quantification is required
- Laboratories validating methods and inter-laboratory studies using the specified precision and trueness checks
Practical benefits include standardized sample preparation, matrix separation to reduce interferences, and traceable ICP‑AES quantification for consistent, comparable results.
Related Standards
- ISO 13547-2: Part 2 - Acid digestion and ICP‑AES method (companion method)
- ISO 12743:2006 - Sampling procedures for concentrates
- ISO 9599 - Determination of hygroscopic moisture in analysis samples
- ISO Guide 35 - Reference material certification principles
Keywords: ISO 13547-1:2014, arsenic determination, ICP‑AES, iron hydroxide coprecipitation, sulfide concentrates, copper sulfide, lead sulfide, zinc sulfide, nickel sulfide, analytical standard.