Determination of Elemental Impurities in Copper Sulfate using ICP-OES

Importance of the topic

In electronic manufacturing, high-purity copper sulfate electrolyte is crucial for optimal conductivity. Trace metal impurities co-deposited during electroplating can degrade performance and reliability of electronic components. Accurate quantification of these impurities ensures consistent product quality and reduces failure rates.

Study objectives and overview

This application note evaluates the Agilent 5800 Vertical Dual View (VDV) ICP-OES, coupled with ICP Expert Pro software, for the rapid multi-element determination of trace impurities in electronic-grade CuSO4. Key goals include streamlining method development, enhancing sample throughput, and demonstrating robust analytical performance across different CuSO4 batches.

Methodology and Instrumentation

• Sample preparation: Three commercial anhydrous CuSO4 samples were dissolved to prepare 2% (w/v) solutions in 18.2 MΩ·cm deionized water. Spike recovery tests used 50 µg/L and 200 µg/L additions.
• Calibration: Single-element standards (5–1000 µg/L) were matrix-matched in 2% CuSO4. Calibration curves were linear (R² 0.9992–1.0000) for all analytes.
• Instrumentation: Agilent 5800 VDV ICP-OES with SeaSpray nebulizer, double-pass cyclonic spray chamber, Easy-fit VDV torch, and SPS 4 autosampler. ICP Expert Pro software provided IntelliQuant Screening, Intelligent Rinse, Early Maintenance Feedback, and automatic background correction (Fitted Background Correction and FACT).

Main results and discussion

• Method detection limits ranged from 0.08 µg/L (Cd, Mn) to 8.43 µg/L (Ca), based on 3σ of blank replicates.
• Spike recovery in CuSO4 sample 1 was within ±10% for all elements; QC precision (%RSD) was <1% for most analytes, <2.5% for Sn.
• Intelligent Rinse reduced average rinse time dynamically, increasing sample throughput by 26% (130 vs. 103 samples in five hours) without compromising data quality.
• Instrument stability over a five-hour run (138 measurements) showed all QC recoveries within ±10% without recalibration.

Benefits and practical applications

• Single-run, multi-element analysis simplifies quality control of plating electrolytes.
• Smart software tools accelerate method setup, reduce argon consumption, and guide wavelength selection.
• Automated background correction and maintenance alerts improve data integrity and minimize downtime.

Future trends and opportunities

• Incorporating AI-driven spectral deconvolution and predictive maintenance could further enhance detection limits and laboratory efficiency.
• Remote monitoring and cloud-based diagnostics may extend uptime and support high-volume production environments.
• Adaptation of this ICP-OES workflow to other high-matrix industrial samples can broaden its impact across electronic materials and related fields.

Conclusion

The Agilent 5800 VDV ICP-OES with ICP Expert Pro delivers a reliable, high-throughput solution for determining elemental impurities in copper sulfate. Smart analysis features streamline method development, boost sample throughput, and ensure stable, accurate results—ideal for electronic materials quality control.

References

1. Miura, S.; Honma, H. Advanced Copper Electroplating for Application of Electronics. Surf. Coat. Technol. 2003, 169–170, 91–95.
2. Agilent Technologies. ICP Expert Software: Powerful software with smart tools for ICP-OES; Publication 5994-1517EN.
3. Agilent Technologies. IntelliQuant Screening: Smarter and quicker semiquantitative ICP-OES analysis; Publication 5994-1518EN.
4. Agilent Technologies. Intelligent Rinse: Increase productivity and reduce errors; Publication 5991-8456EN.