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Monitoring for trace anion contamination in the extracts of electronic components

Applications | 2017 | Thermo Fisher ScientificInstrumentation
Ion chromatography
Industries
Materials Testing, Semiconductor Analysis
Manufacturer
Thermo Fisher Scientific

Summary

Importance of the Topic


The extraction and measurement of trace anion contaminants from electronic components is critical for ensuring the reliability and performance of devices such as disk drives. Moisture combined with residual anions like chloride or sulfate can lead to acid formation and corrosion at sensitive interfaces, causing failures in high-precision components. Ion chromatography provides a sensitive and selective tool for quantifying these ions at ppb levels, supporting quality control and failure analysis.

Objectives and Overview


This study demonstrates two ion chromatography approaches—direct injection and preconcentration—to detect trace levels of common inorganic anions and low–molecular-weight organic acids in water extracts of disk drive components. The goal is to optimize method sensitivity, selectivity, and throughput for routine monitoring of fluoride, chloride, bromide, nitrate, sulfate, phosphate, acetate, formate, acrylate, methacrylate, benzoate, and oxalate.

Methodology and Used Instrumentation


  • Sample Extraction: Disk drive parts soaked in high-purity water at 85 °C for 1 h
  • Direct Injection: 1 mL extract loaded via an autosampler loop
  • Preconcentration: 5 mL extract loaded onto a TAC-LP1 concentrator column

All separations used a Thermo Scientific Dionex ICS-2500 (or ICS-5000+/Integrion) with IonPac AS17/AG17 analytical and guard columns, EG50 KOH eluent generator, ASRS ULTRA suppressor, and suppressed conductivity detection in recycle mode. A gradient from 0.3 mM to 40 mM KOH at 0.5 mL/min and 30 °C ensured separation of weakly and strongly retained anions.

Main Results and Discussion


  • Preconcentration improved sensitivity 3–5× over direct injection, achieving MDLs down to 0.024 µg/L for fluoride and 0.028 µg/L for sulfate
  • Blank levels for most analytes were below 1 µg/L; acetate and formate blanks were slightly higher due to vial and container handling
  • Extract analyses of aluminum spacers and stainless-steel clamps revealed anion levels below 10 µg/L for most targets; oxalate reached 46 µg/L in steel clamp extracts, reflecting cleaning processes
  • Gradient generated by EG50 Eluent Generator showed minimal baseline shifts (<200 nS) and high retention time reproducibility

Practical Benefits and Applications


The described IC methods enable reliable trace anion profiling for electronic component cleanliness, reducing corrosion and head-to-disk failures. They support incoming inspection, process optimization, and failure analysis across printed circuit boards, wafers, and disk drive parts, balancing sensitivity and throughput with minimal eluent waste.

Future Trends and Possibilities for Application


  • Integration of higher capacity concentrator columns and advanced suppressors for even lower detection limits
  • Automation of sample preparation and inline extraction to minimize contamination risk and improve reproducibility
  • Application of similar workflows to emerging components in MEMS, photonics, and battery electrodes
  • Implementation of real-time monitoring of rinsing or cleaning processes via online IC systems

Conclusion


Two complementary IC methods—direct injection and preconcentration—provide robust, sensitive quantitation of trace anions in electronic component extracts. Optimal instrumentation and stringent contamination control ensure MDLs in the sub-ppb range, enabling proactive quality assurance and corrosion prevention in high-reliability electronics manufacturing.

References


  1. Kaiser E Riviello J Rey M Statler J Heberling S J Chromatogr 1997 789 149–155
  2. Liu Y Kaiser E Avdalovic N Microchem J 1999 62 162–173
  3. MacDougall D Crummett WB Anal Chem 1980 52 2242–2249

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