Overview
ISO/TS 13899-1:2004 specifies an inductively coupled plasma atomic emission spectrometric (ICP‑AES) method for the determination of molybdenum (Mo) in alloyed steel. The procedure covers sample dissolution, fuming and dilution, and ICP‑AES measurement using matrix‑matched calibration and optional internal standardization. The method is applicable for Mo mass fractions from 0.03 % to 8.5 %.
Keywords: ISO/TS 13899-1, molybdenum determination, ICP‑AES, steel analysis, alloyed steel, molybdenum content.
Key topics and technical requirements
- Analytical principle: Dissolution of a 0.25 g test portion in hydrochloric, nitric and phosphoric acids; perchloric fuming; treatment with hydrofluoric acid; dilution and nebulization into ICP‑AES.
- Matrix matching and bracketing: Calibration solutions must closely match the sample matrix and bracket the sample concentration to compensate spectral and matrix interferences. If sample composition is unknown, a semi‑quantitative pre‑analysis is required.
- Instrument performance criteria:
- Bandwidth (FWHM) for selected lines < 0.030 nm
- Short‑term stability (RSD of 10 measurements) ≤ 0.4%
- Background equivalent concentration (BEC) < 0.5 mg/L
- Detection limit (DL) < 0.015 mg/L
- Calibration linearity: correlation coefficient > 0.999
- Recommended analytical lines & interferences: examples include Mo 202.03 nm (Ta interference) and Mo 281.61 nm (Al, Hf interference); scandium 363.07 nm is recommended as an interference‑free internal standard line for many matrices.
- Reagents and apparatus: Analytical‑grade acids (HCl, HNO3, H3PO4, HClO4, HF), class A volumetric glassware, HF‑resistant nebulizer/spray system and PTFE beakers.
Applications and users
This technical specification is intended for:
- Steel producers and alloy manufacturers for quality control of Mo content
- Analytical and metallurgical laboratories performing compositional analysis of alloyed steels
- Third‑party testing and certification bodies requiring standardized Mo quantification
- R&D groups developing or validating ICP‑AES methods for high‑alloy steels
Practical applications include batch release testing, alloy verification, traceability in supply chains, and support for metallurgical process control where accurate Mo content is critical to material properties.
Related standards
- ISO/TS 13899 (Parts 2 & 3) - determination of Nb and W by ICP‑AES
- ISO 14284 - sampling and sample preparation for chemical composition
- ISO 3696 - water for analytical laboratory use
- ISO 648, ISO 1042 - calibrated pipettes and volumetric flasks
- ISO 5725 series - accuracy (trueness and precision) of measurement methods
Using ISO/TS 13899-1 helps ensure reproducible, accurate molybdenum determinations in alloyed steels and supports compliance with international analytical best practices.