Overview
ASTM E168-16(2023), titled Standard Practices for General Techniques of Infrared Quantitative Analysis, is a key ASTM standard for laboratories and industries utilizing infrared (IR) spectroscopy for quantitative chemical analysis. Developed by ASTM Committee E13 on Molecular Spectroscopy and Separation Science, this standard provides comprehensive guidelines suitable for both novices seeking a foundational overview and experienced practitioners needing a refresher on less frequently used procedures.
ASTM E168 covers best practices for the preparation, operation, and calculation techniques pertinent to quantitative IR analysis. It includes instructions for both computerized data collection as well as traditional, non-computer-based methods. The scope makes it a versatile resource for users of all IR instrument types including dispersive, filter, prism, and Fourier transform infrared (FT-IR) spectrometers.
Key Topics
- Infrared Quantitative Analysis Techniques: Practical steps for optimizing the accuracy and reliability of quantitative IR measurements, including instrument stability, sample preparation, and selection of analytical wavenumbers.
- Calibration and Baselines: Guidance on how to prepare calibration curves, use of baselines, and the importance of bracketing analyte concentrations for accurate calibration and analysis.
- Single vs. Multicomponent Analysis: Procedures for applying Beer’s Law to both single analyte and complex mixtures, including matrix inversion and least-squares regression for determining concentrations in multicomponent samples.
- Sample Types and Preparation: Detailed recommendations for handling liquids, solids, and gases, addressing specific challenges such as intermolecular interactions, path length requirements, and pressure conditions for gaseous samples.
- Error Sources and Statistical Evaluation: Discussion of systematic (determinate) and random (indeterminate) errors, along with statistical approaches to evaluate bias, precision, and standard deviation in quantitative IR analysis.
- Safety and Compliance: Emphasis on user responsibility for implementing appropriate safety, health, and regulatory practices associated with the chemicals, instrumentation, and procedures used.
Applications
This standard is applicable wherever infrared spectroscopy is used for quantitative chemical analysis, including:
- Quality Control in Manufacturing: Routine and validation testing in polymer, pharmaceutical, petrochemical, and food industries.
- Research and Development: Advanced material characterization, reaction monitoring, and process optimization.
- Environmental Analysis: Determination of pollutants or trace-level contaminants in air, water, and soil using IR quantitative techniques.
- Forensics and Regulatory Compliance: Reliable, standardized protocols for evidentiary analysis and adherence to industry and government regulation.
Users benefit from ASTM E168 by improving measurement reliability, ensuring consistency across laboratories, and facilitating data comparisons. The standard’s stepwise instructions on calibration, baseline subtraction, and error analysis enhance both accuracy and reproducibility in IR spectroscopic measurements.
Related Standards
For broader implementation and best practices, ASTM E168 is referenced alongside several other important ASTM standards, including:
- ASTM E131: Terminology Relating to Molecular Spectroscopy
- ASTM E334: General Techniques of Infrared Microanalysis
- ASTM E932: Describing and Measuring Performance of Dispersive Infrared Spectrometers
- ASTM E1252: Obtaining Infrared Spectra for Qualitative Analysis
- ASTM E1421: Measuring Performance of Fourier Transform Mid-Infrared (FT-MIR) Spectrometers
- ASTM E1655: Practices for Infrared Multivariate Quantitative Analysis
Consulting these related standards in conjunction with ASTM E168 ensures comprehensive adherence to best practices in IR spectroscopy, from instrument validation and data acquisition to advanced multivariate calibration methods.
Keywords: ASTM E168, infrared quantitative analysis, IR spectroscopy, Beer’s Law, calibration, baseline correction, quantitative chemical analysis, instrument performance, sample preparation, ASTM standards.