Agilent ICP-MS Journal (September 2010 – Issue 43)

Význam tématu

Atomic spectrometry techniques such as AAS, ICP-OES and ICP-MS are cornerstone methods for elemental analysis across diverse fields including environmental monitoring, materials science and quality control. Their high sensitivity, broad dynamic range and multi-element capabilities enable reliable quantification of trace metals and metalloids. Monitoring of brominated flame retardants (BFRs) in plastics is critical due to regulatory limits and concerns over toxicity and environmental persistence.

Cíle a přehled studie / článku

This issue of the Agilent ICP-MS Journal profiles the expanded atomic spectrometry portfolio following Agilent’s acquisition of Varian, and presents a user application for determining polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in polymeric materials. The goal is to highlight new instrumentation offerings and demonstrate a robust HPLC-ICP-MS method for accurate BFR quantification in a certified reference material.

Použitá instrumentace

Key systems described or employed:

• Flame AAS: Varian AA240 FS, AA280 FS with Fast Sequential capability
• Graphite Furnace AAS: Varian GTA 120 furnace accessory; AA240 and AA280 Zeeman GFAAS
• ICP-OES: Varian 700-ES series (710/715-ES, 720/725-ES, 730/735-ES) in radial and axial configurations
• ICP-MS: Agilent 4500, 7500 and 7700 Series; 7700e, 7700x and 7700s with ORS3 and HMI options
• HPLC-ICP-MS coupling: Agilent 1100 HPLC system linked to Agilent 7500ce ICP-MS

Použitá metodika

Sample preparation utilized accelerated solvent extraction (ASE) of cryogenically ground polypropylene reference material (ERM-EC591) with toluene at 90 °C. Extracts were spiked with 9-bromoanthracene as internal standard and separated on a Phenomenex Luna phenyl-hexyl column using a methanol gradient. The ICP-MS was operated with cooled spray chamber (–5 °C), elevated RF power, oxygen addition and helium collision gas in the ORS3 cell. MassHunter software Revision provided integrated Startup, Hardware, Batch, Queue and Data Analysis panes for streamlined instrument control and routine sequencing.

Hlavní výsledky a diskuse

Chromatographic separation achieved baseline resolution of PBDE congeners (47, 183, 206, 209) and PBB-209. Total bromine measurement via peak area summation matched the certified value of 2.08 g/kg (recovery 102 %, RSD 2.5 %, n = 6). Individual recoveries for PBDE-47, ‑183, ‑209 and PBB-209 ranged from 93.6 % to 105.7 % with RSDs below 7 %. Lower recovery for PBDE-206 (70 %) is attributed to reference uncertainty and potential in-line ^79Br^+ back-conversion in GC but was consistent with the HPLC-ICP-MS approach.

Přínosy a praktické využití metody

• The HPLC-ICP-MS method operates at ambient temperature, mitigating thermal debromination typical in GC-based analysis.
• ASE extraction ensures efficient recovery while preserving analyte integrity.
• MassHunter’s standardized Batch and Pre-set Method workflows simplify multi-element quantification and quality control in high-throughput labs.
• High Matrix Introduction (HMI) and ORS3 cell capabilities extend matrix tolerance and interference removal in complex polymer extracts.

Budoucí trendy a možnosti využití

Advances in integrated atomic spectrometry will focus on:

• Enhanced collision/reaction cell chemistries for tailored interference suppression.
• Further automation of sample introduction, tuning and performance monitoring via advanced software interfaces.
• Expansion of speciation and screening techniques combining full-spectrum acquisition (Quick Scan) with quantitative methods.
• Increased adoption of coupled techniques (LC-MS/ICP-MS) for comprehensive molecular and elemental profiling in complex matrices.

Závěr

The integration of Varian’s AAS and ICP-OES portfolio into Agilent’s leading ICP-MS platform creates a versatile suite of atomic spectrometry instruments. The demonstrated HPLC-ICP-MS methodology offers reliable, high-throughput determination of brominated flame retardants in plastics, meeting regulatory requirements while addressing analytical challenges such as debromination and matrix effects.

Reference

1. Commission Decision 2005/618/EC. Off. J. Eur. Comm. L 214, 65 (2005).
2. T. P. J. Linsinger, S. Voorspoels, A. Liebich; Anal. Bioanal. Chem. 390, 399 (2008).
3. R. Zeleny et al.; Anal. Bioanal. Chem. 369, 1501 (2010).