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A Consolidated Approach for Analytical Testing of Recycled Industrial Plastics

Others | 2022 | WatersInstrumentation
GC/MSD, GC/MS/MS, Pyrolysis, GC/QQQ, GC/API/MS, LC/MS, LC/MS/MS, LC/QQQ, GPC/SEC
Industries
Energy & Chemicals
Manufacturer
Waters

Summary

Significance of Topic


Polyamide recycling addresses critical needs in the automotive and plastics industries by reducing CO₂ emissions, conserving resources and supporting circular economy goals. High-performance polymers, such as Nylon-based materials, can replace heavier metal components, but consistent quality and safety must be maintained when reusing or reprocessing scrap materials.

Study Objectives and Overview


This case study evaluates a comprehensive analytical workflow to compare virgin and post-industrial recycled polyamide (PrestaMID™) pellets and molded worm gear parts. The goals are to characterize thermal, molecular, mechanical and chemical differences as a function of regrind content (0–100%), and to determine how recycled content affects component performance.

Methodology and Instrumentation


A multi‐technique approach was used:
  • Thermogravimetric Analysis (TGA) to assess thermal degradation profiles.
  • Differential Scanning Calorimetry (DSC) and Modulated DSC (MDSC) for melting/crystallization behavior and enthalpic relaxation.
  • Size-Exclusion Chromatography (SEC/GPC) using HFIP mobile phase and ACQUITY APC XT columns to measure molecular weight distribution.
  • Pyrolysis-Atmospheric Pressure GC-High Resolution MS (py-APGC-HRMS) with ToF detection and UNIFI™ software for chemical fingerprinting and multivariate marker identification.

Key Results and Discussion


TGA showed that gears and pellets with 100% recycled content decomposed at temperatures ~10–20 °C lower than virgin samples, indicating reduced thermal stability. DSC data revealed nearly identical melting points across all blends, while enthalpic recovery increased with regrind percentage, suggesting higher brittleness risk. SEC/GPC demonstrated a 24% drop in peak molecular weight (from 126 kDa to 97 kDa) and broader distribution for fully recycled gears. Py-APGC-HRMS combined with PCA and S-plot analyses identified unique pyrolyzate markers in recycled samples, such as N-vinylcaprolactam, aiding targeted chemical monitoring.

Benefits and Practical Applications


The consolidated analytical protocol enables manufacturers to:
  • Quantify the impact of recycled content on thermal and mechanical properties.
  • Detect chemical markers that differentiate virgin vs. recycled polymers.
  • Optimize regrind proportions without compromising component safety.
  • Support compliance strategies for future regulations on recycled plastic quotas.

Future Trends and Applications


Advances may include automated multivariate monitoring, expansion to other polymer families, integration with real-time process controls and development of harmonized standards. Emerging high-throughput calorimetric and chromatography platforms could streamline quality checks in closed-loop recycling.

Conclusion


This integrated analytical framework demonstrates that combining thermal analysis, advanced SEC, and soft-ionization HRMS provides a robust basis for assessing recycled polyamide performance. Such a strategy supports safe automotive applications and advances industrial recycling targets.

Reference


1. Recycling International (2012) Study proves green potential of recycled polyamide.
2. EuRIC (2021) Position paper on ELV and 3R type approval Directives.
3. Rethmann C. (2022) Master’s thesis on polymer recycling in automotive safety components.
4. TA Instruments (TA454) Nonisothermal Crystallization Kinetics Application Note.
5. Wudy K. & Drummer D. (2018) Aging effects of PA12 in selective laser sintering. Additive Manufacturing 25.
6. Nasa JL et al. (2020) Analytical pyrolysis techniques for plastics in heritage science. Molecules 25(1705).
7. Stevens DM et al. (2012) Detection of extractable compounds from polymers. Waters Application Note 720004211.

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