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POLYMER ANALYSIS | TESTING


Chemometric analysis of the presence of different


plasticisers in PVC using the Agilent 4500 FTIR and method developed by Actus Analytical


Source: Actus Analytical


see deeper inside a polymer material if the material is transparent to the laser. “Using confocal depth profiling, you can take a series of Raman spectra through the material and then visualiae the image in three dimensions,” explains Bradley. This technique can be used, for example, to examine fiber or filler dispersion through the bulk polymer.


Phthalate analysis It is becoming increasingly important today to be able to measure and document the absence of chemicals of concern. Phthalate-based plasticicers, for instance, have been commonly used in flexible PVC but concerns about orthophthalates have led to regulatory restrictions, leading to the need to be able to identify their presence. Actus Analytical has developed an FTIR method to screen polymer samples and detect orthophthalate plasticiser down to levels of 0.1% (1000 ppm), according to Michael Gray, CEO of Actus Analytical. The method is positioned as a quality control tool to allow processors to quickly determine whether or not a sample contains an orthophthalate. FTIR is well suited for such quality control tasks, Gray says, because it is a non-destructive, simple, and inexpensive test that gives immediate results. In addition, the chemometric model allows its use by non-technical personnel. The technique was developed for the Agilent 4500 FTIR, which he says is very well suited to the task due to its power and patented permanent calibration. “There are approximately 21 orthophthalates, but only 10 of these have ever been made in significant volumes, five to eight of which are banned by various regulations,” says Gray. The Actus method takes an FTIR spectrum and looks for characteristic vibrational responses of an orthophthalate within the sample, using chemometric modeling with algorithms that


46 COMPOUNDING WORLD | January 2020


compare the spectra to reference libraries. “Because we can detect below 1000ppm, which is the legal limit in restricted cases, we don’t have any ‘false negatives’—if no orthophthalate is detected then it contains no orthophthalate,” says Gray. The method can distinguish between


orthophthalates and other phthalates (terephthalates or isophthalates, for example) as well as other classes of plasticisers (including adipates and citrates). While FTIR can quantify the level of orthophthalate, it cannot distinguish between different types of orthophthalates (the speciation). However, screening with FTIR allows analysts to determine what samples may need further testing by gas chromatography (GC)-mass spectrometry (MS), if desired, to determine which of the orthophthalates is present and to affirm their concentration.


Paperless laboratories Digitisation—the move from paper to digital data— takes effort but offers the potential for reduced error, improved data security, automation, and higher efficiency. Anton Paar has introduced AP Connect, which connects all laboratory devices to one software system that serves as the main data link for transferring lab data to a central database and data management system. The software supports all the company’s devices, including viscometers and dynamic-mechanical analysis (DMA) devices, as well as selected third-party devices. Automated testing equipment is more accurate


and efficient than manual methods. For example, robotic testing equipment and software program from LabsCubed automatically collects and analyses physical property data from sets of samples. The automated program can be used to speed material development by making testing, data collection, and data analysis more efficient,


www.compoundingworld.com


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