How did FILAB help a customer distinguish between the polymer materials polyamide PA 6 and PA 6.6?
Polyamide polymers, more commonly known as nylons, are widely used in many industries. PA 6 and PA 6.6 polyamide polymers are the most commonly used. Although they have many similarities, they differ in certain characteristics (mechanical properties, chemical structures, water absorption, and thermal resistance) that make them suitable for specific applications.
This case study focuses on the method and technical means used to determine whether a polyamide is PA6 or PA6.6.
Context
Our client called on FILAB to help with a production discrepancy. One of their machines had been mistakenly fed with the wrong raw material. They wanted to take samples from 130,000 parts throughout the production process to determine whether they were made of PA 6.6 (compliant) or PA 6 (non-compliant).
The client commissioned FILAB, a laboratory specializing in material characterization and chemical analysis, to first identify the polymers and then restart production.
Determination of the chemical nature of parts
What analysis techniques did the laboratory decide to use to distinguish between the two polyamide polymers?
DSC analysis
DSC is a thermal analysis technique that measures the differences in heat exchange between a sample to be analyzed and a control (a reference).
In this case, it made it possible to identify the characteristic temperatures of each polymer. The analysis revealed that the sample analyzed was indeed PA 6.6, consistent with normal production.
Pyrolysis GC-MS analysis
This technique confirmed the nature of the polymer found. Pyrolysis coupled with mass spectrometry (Py-GC-MS) is a pyrolysis technique followed by gas chromatography coupled with mass spectrometry (GC-MS) that identifies the organic compounds in a sample and determines its chemical composition by breaking it down into its volatile components.
The nature of the polymer was thus confirmed.
Conclusion of the study
FILAB's in-depth analysis made it possible to determine with precision that the parts manufactured and analyzed complied with our client's specifications. This information was essential for successfully restarting production.
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Frequently asked questions
How can PA 6 polyamide be distinguished from PA 6.6 in the laboratory?
FILAB combined DSC thermal analysis and pyrolysis GC-MS to distinguish between the two polyamides. DSC provides information on characteristic thermal transitions, while pyrolysis GC-MS enables chemical identification of the matrix. In this study, the results confirmed the presence of PA 6.6 in the parts analyzed.
Why is DSC useful for identifying a polyamide?
DSC measures the heat exchanges of a sample during a thermal program. The observed transitions, including melting, help distinguish polyamide families. In the case presented, the thermal profile was consistent with PA 6.6. However, its interpretation must take into account the material’s formulation and thermal history.
What does pyrolysis GC-MS add to DSC?
Pyrolysis GC-MS characterizes the products resulting from the polymer’s thermal decomposition. Their separation and identification make it possible to recognize characteristic fragments of the matrix. In this study, this approach confirmed the identification obtained by DSC and strengthened the distinction between PA 6 and PA 6.6.
How can production be checked after a raw material mix-up?
The inspection is based on a sampling plan defined according to the production history and the risk of mixing. In this study, the client wanted to examine samples taken from a production run of 130,000 parts. The analysis identified the material of the parts received and provided data to determine the appropriate action for the batch.
Are compliant samples sufficient to declare all parts in the batch compliant?
The compliance of the samples analyzed provides direct information about those parts. Extending this conclusion to the entire batch depends on the representativeness of the sampling plan and the acceptance criteria selected. In this study, FILAB confirmed the presence of PA 6.6 in the parts examined, providing the client with information to organize the resumption of production.