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Carbon and Sulfur Determination in High Carbon Ferroalloys - CS744

Applications | 2019 | LECOInstrumentation
Elemental Analysis, Thermal Analysis
Industries
Materials Testing, Energy & Chemicals
Manufacturer
LECO

Summary

Importance of the Topic


Accurate determination of carbon and sulfur in high-carbon ferroalloys is essential for steel and cast iron production. Carbon defines key mechanical properties and alloying behavior, while sulfur is a detrimental impurity that can compromise strength and toughness. Reliable analysis supports quality control and ensures consistent metallurgical performance.

Objectives and Study Overview


This application note presents a validated procedure for simultaneous measurement of carbon and sulfur in high-carbon ferroalloys using a LECO CS744 combustion analyzer. The study aims to optimize accelerator mixtures, establish calibration protocols, and demonstrate method accuracy and precision under routine laboratory conditions.

Methodology and Instrumentation


Sample Preparation
  • Grind or select a representative powder or granular ferroalloy sample.
  • Use ceramic crucibles preheated at 1350 °C for 20 min or 1000 °C for 40 min, then store in a desiccator.
  • Accelerator Mixture
    • 0.4 g LECO iron powder
    • 0.6 g vanadium pentoxide (V2O5)
    • 1.5 g LECOCEL
    Analysis Parameters
    • Purge time: 10 s
    • Analysis delay: 20 s
    • Furnace mode: constant at 100 % power
    • Integration time: 40–70 s
    • Comparator level: 1.00 % for both elements
    • Significant digits: 5
    Procedure Steps
    • Run three blank replicates to establish baseline.
    • Calibrate with at least two reference materials (e.g., NIST, LECO CRM standards) in triplicate.
    • Analyze samples in replicates, applying blank subtraction and drift correction as per instrument manual.

    Main Results and Discussion


    Calibration using NIST 64c and BCS 204/4 ferro-chromium standards yielded linear responses forced through the origin. Typical results for a ~0.25 g sample:
    • Reference NIST 64c: 4.698 ± 0.040 % C, 0.0673 ± 0.0034 % S
    • BCS 204/4: 5.620 ± 0.015 % C, 0.0101 ± 0.0002 % S
    Precision and accuracy met industrial QC requirements. The V2O5-LECOCEL mixture improved sulfur recovery, and the consistent blank enabled reliable subtraction.

    Practical Benefits and Applications


    The described CS744 method offers:
    • Rapid turnaround for routine quality control in ferroalloy and steel plants
    • High analytical precision and accuracy for carbon and sulfur
    • Robust performance with minimal sample preparation variability

    Future Trends and Potential Applications


    Emerging developments may include
    • Automation with autoloaders for higher throughput
    • Alternative, less hazardous accelerators
    • Integration of real-time data analytics for process control

    Conclusion


    The CS744 combustion analysis protocol provides a reliable, precise, and accurate method for carbon and sulfur determination in high-carbon ferroalloys. Its robust calibration and accelerator strategy ensure consistency for industrial QC environments.

    Instrument Used


    • LECO CS744 Carbon/Sulfur Analyzer with induction furnace

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